Corrosion of metals and alloys - Aqueous corrosion testing of zirconium alloys for use in nuclear power reactors (ISO 10270:2022)

This document specifies:
a) the determination of mass gain;
b) the surface inspection of products of zirconium and its alloys when corrosion is tested in water at
360 °C or in steam at or above 400 °C;
c) the performance of tests in steam at 10,3 MPa.
This document is applicable to wrought products, castings, powder metallurgy products and weld
metals.
This method has been widely used in the development of new alloys, heat-treating practices and for
the evaluation of welding techniques. It is applicable for use in its entirety to the extent specified for a
product acceptance test, rather than merely a means of assessing performance in service.

Korrosion von Metallen und Legierungen - Korrosionsprüfung in wässrigen Lösungen für in Kernreaktoren angewendete Zirkoniumlegierungen (ISO 10270:2022)

Diese Internationale Norm legt fest:
a) die Bestimmung der Massezunahme;
b) die Untersuchung der Oberflächen von Produkten aus Zirkonium und Zirkoniumlegierungen nach einer Korrosionsprüfung in Wasser bei 360 °C oder in Dampf bei oder über 400 °C;
c) dass die Prüfungen in Dampf unter einem Druck von 10,3 MPa (1 500 psi) durchzuführen sind.
Diese Internationale Norm ist auf warm verformte Produkte, Gussteile, pulvermetallurgische Produkte und Schweißgut anwendbar.
Das beschriebene Verfahren wurde bereits vielfach zur Entwicklung neuer Legierungen und Wärmebehandlungsverfahren sowie zur Bewertung von Schweißverfahren genutzt und sollte nicht nur zur Beurteilung des Betriebsverhaltens angewendet werden, sondern stattdessen in seiner Gesamtheit, in dem Umfang, der zur Abnahmeprüfung des jeweiligen Produkts festgelegt ist.

Corrosion des métaux et alliages - Essais de corrosion aqueuse des alliages de zirconium utilisés dans les réacteurs nucléaires (ISO 10270:2022)

Le présent document décrit :
a) la détermination du gain en masse ;
b) le contrôle superficiel des produits en zirconium et en alliages de zirconium après essai de corrosion dans l'eau à 360 °C et dans la vapeur à 400 °C ou plus ;
c) les performances des essais dans la vapeur à 10,3 MPa.
Le présent document est applicable aux produits corroyés, moulés, aux produits de la métallurgie des poudres et aux métaux d'apport pour le soudage.
La méthode a été beaucoup utilisée pour mettre au point de nouveaux alliages et de nouvelles techniques de traitement thermique et à évaluer les techniques de soudage Elle peut être utilisée dans sa totalité comme moyen de réception des produits plutôt que comme moyen d'évaluation de leurs propriétés en service.

Korozija kovin in zlitin - Preskušanje vodne korozije cirkonijevih zlitin za uporabo v jedrskih reaktorjih (ISO 10270:2022)

Ta dokument določa: a) določevanje povečanja mase; b) pregledovanje površine proizvodov iz cirkonija in njegovih zlitin pri preskušanju korozije v vodi pri temperaturi 360 °C ali v pari pri temperaturi 400 °C ali več; c) izvajanje preskusov v pari pri tlaku 10,3 MPa. Ta dokument se uporablja za gnetene zlitine, ulitke, proizvode, izdelane z metalurgijo prahu, in zvarne kovine. Ta metoda se pogosto uporablja pri razvoju novih zlitin, v postopkih toplotne obdelave in za vrednotenje tehnik varjenja. V obsegu, določenem za preskus sprejemljivosti proizvoda, se lahko uporablja v celoti in ne zgolj kot sredstvo za ocenjevanje učinkovitosti delovanja.

General Information

Status
Published
Public Enquiry End Date
19-Nov-2020
Publication Date
02-Mar-2022
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
02-Mar-2022
Due Date
07-May-2022
Completion Date
03-Mar-2022

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SLOVENSKI STANDARD
SIST EN ISO 10270:2022
01-april-2022
Nadomešča:
SIST EN ISO 10270:2008

Korozija kovin in zlitin - Preskušanje vodne korozije cirkonijevih zlitin za uporabo

v jedrskih reaktorjih (ISO 10270:2022)

Corrosion of metals and alloys - Aqueous corrosion testing of zirconium alloys for use in

nuclear power reactors (ISO 10270:2022)

Korrosion von Metallen und Legierungen - Korrosionsprüfung in wässrigen Lösungen für

in Kernreaktoren angewendete Zirkoniumlegierungen (ISO 10270:2022)
Corrosion des métaux et alliages - Essais de corrosion aqueuse des alliages de
zirconium utilisés dans les réacteurs nucléaires (ISO 10270:2022)
Ta slovenski standard je istoveten z: EN ISO 10270:2022
ICS:
27.120.99 Drugi standardi v zvezi z Other standards related to
jedrsko energijo nuclear energy
77.060 Korozija kovin Corrosion of metals
SIST EN ISO 10270:2022 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST EN ISO 10270:2022
---------------------- Page: 2 ----------------------
SIST EN ISO 10270:2022
EN ISO 10270
EUROPEAN STANDARD
NORME EUROPÉENNE
February 2022
EUROPÄISCHE NORM
ICS 27.120.10; 77.060 Supersedes EN ISO 10270:2008
English Version
Corrosion of metals and alloys - Aqueous corrosion testing
of zirconium alloys for use in nuclear power reactors (ISO
10270:2022)

Corrosion des métaux et alliages - Essais de corrosion Korrosion von Metallen und Legierungen -

aqueuse des alliages de zirconium utilisés dans les Korrosionsprüfung in wässrigen Lösungen für in

réacteurs nucléaires (ISO 10270:2022) Kernreaktoren angewendete Zirkoniumlegierungen

(ISO 10270:2022)
This European Standard was approved by CEN on 26 December 2021.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this

European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references

concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN

member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by

translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management

Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 10270:2022 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN ISO 10270:2022
EN ISO 10270:2022 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

---------------------- Page: 4 ----------------------
SIST EN ISO 10270:2022
EN ISO 10270:2022 (E)
European foreword

This document (EN ISO 10270:2022) has been prepared by Technical Committee ISO/TC 156

"Corrosion of metals and alloys" in collaboration with Technical Committee CEN/TC 262 “Metallic and

other inorganic coatings, including for corrosion protection and corrosion testing of metals and alloys”

the secretariat of which is held by BSI.

This European Standard shall be given the status of a national standard, either by publication of an

identical text or by endorsement, at the latest by August 2022, and conflicting national standards shall

be withdrawn at the latest by August 2022.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN ISO 10270:2008.

Any feedback and questions on this document should be directed to the users’ national standards

body/national committee. A complete listing of these bodies can be found on the CEN website.

According to the CEN-CENELEC Internal Regulations, the national standards organizations of the

following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,

Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,

Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of

North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the

United Kingdom.
Endorsement notice

The text of ISO 10270:2022 has been approved by CEN as EN ISO 10270:2022 without any modification.

---------------------- Page: 5 ----------------------
SIST EN ISO 10270:2022
---------------------- Page: 6 ----------------------
SIST EN ISO 10270:2022
INTERNATIONAL ISO
STANDARD 10270
Second edition
2022-02
Corrosion of metals and alloys —
Aqueous corrosion testing of
zirconium alloys for use in nuclear
power reactors
Corrosion des métaux et alliages — Essais de corrosion aqueuse des
alliages de zirconium utilisés dans les réacteurs nucléaires
Reference number
ISO 10270:2022(E)
© ISO 2022
---------------------- Page: 7 ----------------------
SIST EN ISO 10270:2022
ISO 10270:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on

the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below

or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
© ISO 2022 – All rights reserved
---------------------- Page: 8 ----------------------
SIST EN ISO 10270:2022
ISO 10270:2022(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ..................................................................................................................................................................................... 1

3 Terms and definitions .................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 2

5 Significance ............................................................................................................................................................................................................... 2

6 Interference............................................................................................................................................................................................................... 2

7 Reagents and materials ................................................................................................................................................................................ 2

8 Apparatus .................................................................................................................................................................................................................... 3

9 Hazards .......................................................................................................................................................................................................................... 3

10 Sampling, test specimens and test units .................................................................................................................................... 3

11 Preparation of apparatus ...........................................................................................................................................................................4

12 Calibration and standardization ........................................................................................................................................................4

12.1 High mass gain coupon preparation ................................................................................................................................... 4

12.2 Autoclaves ................................................................................................................................................................................................... 4

12.3 Use of control coupons..................................................................................................................................................................... 7

12.4 Calibration .................................................................................................................................................................................................. 7

13 Conditioning .............................................................................................................................................................................................................7

13.1 Test water quality ................................................................................................................................................................................ 7

13.2 Autoclave load restrictions ......................................................................................................................................................... 8

13.3 Test conditions ........................................................................................................................................................................................ 8

13.3.1 Temperature ........................................................................................................................................................................... 8

13.3.2 Pressure ..................................................................................................................................................................................... 8

13.3.3 Time ............................................................................................................................................................................................... 8

13.3.4 Tests ............................................................................................................................................................................................... 8

13.4 Specimen preparation ...................................................................................................................................................................... 8

13.4.1 Etched specimens .............................................................................................................................................................. 8

13.4.2 As-manufacturer specimens .................................................................................................................................... 8

14 Procedure ....................................................................................................................................................................................................................8

14.1 Inspection of specimens ........................................................................................................................................... ...................... 8

14.2 Dimensions, weight and inspection ..................................................................................................................................... 9

14.3 Autoclaving ................................................................................................................................................................................................ 9

14.3.1 Placing of test specimens ............................................................................................................................................ 9

14.3.2 Venting method A .............................................................................................................................................................. 9

14.3.3 Venting method B ........................................................................................................................................................... 10

14.3.4 Closed system method C ........................................................................................................................................... 10

14.3.5 Refreshed autoclaving, method D .................................................................................................................... 11

14.4 Post-test measurements and inspection ...................................................................................................................... 11

15 Calculation or interpretation of results ...................................................................................................................................11

15.1 Calculation of mass gain ............................................................................................................................................................. 11

15.2 Visual interpretation of surface appearance ............................................................................................................12

15.3 Invalid tests ............................................................................................................................................................................................12

16 Test report ...............................................................................................................................................................................................................12

Annex A (informative) Guide to specimen preparation ...............................................................................................................13

Bibliography .............................................................................................................................................................................................................................16

iii
© ISO 2022 – All rights reserved
---------------------- Page: 9 ----------------------
SIST EN ISO 10270:2022
ISO 10270:2022(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents are noted. This document was drafted in accordance with the editorial

rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject

of patent rights. ISO is not held responsible for identifying any or all such patent rights. Details of any

patent rights identified during the development of the document will be in the Introduction and/or on

the ISO list of patent declarations received (see www.iso.org/patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to

the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see

www.iso.org/iso/foreword.html.

This document was prepared by Technical Committee ISO/TC 156, Corrosion of metals and alloys, in

collaboration with the European Committee for Standardization (CEN) Technical Committee CEN/

TC 262, Metallic and other inorganic coatings, including for corrosion protection and corrosion testing of

metals and alloys, in accordance with the Agreement on technical cooperation between ISO and CEN

(Vienna Agreement).

This second edition cancels and replaces the first edition (ISO 10270:1995), which has been technically

revised. It also incorporates the Technical Corrigendum ISO 10270:1995/Cor 1:1997. The main changes

compared with the previous edition are as follows:
— the references have been updated;

— in Clause 4, two sentences have been added: “The tests in water is performed at 18,6 MPa. The

pressure is also determined by the contractor's requirements.”;

— in 5.2, “the test” has been replaced by “the measurement to avoid erroneous results from differing

corrosion behaviour of the materials”;
— in 7.1, “welding grade” has been replaced by “of purity 999,9 ml/l or higher”,

— in 11.1, d), “1 day” has been replaced by “24 h”; and “at 18,6 MPa” has been added after “at 360 °C in

water”.

— in 12.1, a sentence has been added: “Post-heat treatment, the coupons are inspected for any residual

oxide and prepared (e.g. etched) in line with standard coupons”;

— in 12.3.4, a sentence has been added: “However, for the product acceptance test, it is better to keep

the control coupons as evidence of test effectiveness.”;

— in 13.3.1, “±3 °C for steam tests, and ±6 °C for water tests” has been replaced by “±3 °C for steam

tests and water tests”;
— in 13.3.3, “3 days or 14 days” has been replaced by “72 h or 336 h”;
© ISO 2022 – All rights reserved
---------------------- Page: 10 ----------------------
SIST EN ISO 10270:2022
ISO 10270:2022(E)

— in 14.2, a sentence has been added: “Mass gain measurements are taken in triplicate for each

specimen and a mean value calculated”;

— in 14.3.1, a sentence has been added: “The separators are such as not to induce Galvanic interaction

between the samples and the separators”; “zirconium or zirconium alloy” has been added before

“stainless steel”;

— in Clause 16, “including its number and year of publication” has been added before “this document”;

— in A.3.1, “3 % (m/m) of hydrofluoric acid (7.7), 39 % (m/m) of nitric acid (7.8)” has been replaced by

“40 g/kg ± 20 g/kg of hydrofluoric acid (7.7), 450 g/kg ± 50 g/kg of nitric acid (7.8)”, and a sentence

has been added: “A different acid ratio may be chosen to satisfy the requirement of a smooth and

shining surface given in 13.4.1;
— in A.3.2, “9 % (m/m) ± 1 % (m/m)” has been replaced by “90 g/kg ± 10 g/kg” and
“30 % (m/m) ± 5 % (m/m)” has been replaced by “300 g/kg ± 50 g/kg”;

— in A.4.2,“25 % (V/V)” has been replaced by “250 ml/l” and “50 % (V/V)” has been replaced by

“500 ml/l”;

— in Clause A.6, the following text has been added: “or placed into the oven at a recommended

temperature of 60 °C to 70 °C for 1 h" and “The specimens need to be cooled to room temperature

after removing from the oven”.

Any feedback or questions on this document are directed to the user’s national standards body. A

complete listing of these bodies can be found at www.iso.org/members.html.
© ISO 2022 – All rights reserved
---------------------- Page: 11 ----------------------
SIST EN ISO 10270:2022
---------------------- Page: 12 ----------------------
SIST EN ISO 10270:2022
INTERNATIONAL STANDARD ISO 10270:2022(E)
Corrosion of metals and alloys — Aqueous corrosion
testing of zirconium alloys for use in nuclear power
reactors

WARNING — This document can involve the use of hazardous materials, operations and

equipment (see Clause 9). It is the responsibility of the user of this document to consult and

establish appropriate safety and health practices and determine the applicability of regulatory

limitations prior to use.
1 Scope
This document specifies:
a) the determination of mass gain;

b) the surface inspection of products of zirconium and its alloys when corrosion is tested in water at

360 °C or in steam at or above 400 °C;
c) the performance of tests in steam at 10,3 MPa.

This document is applicable to wrought products, castings, powder metallurgy products and weld

metals.

This method has been widely used in the development of new alloys, heat-treating practices and for

the evaluation of welding techniques. It is applicable for use in its entirety to the extent specified for a

product acceptance test, rather than merely a means of assessing performance in service.

2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
3.1
etching
process for the removal of surface metal by action of acids in water
3.2
control coupon

zirconium alloy specimen of known performance used to monitor the validity of the test

3.3
high mass gain coupon

zirconium alloy specimen that has been specially heat-treated to produce a mass gain higher than the

maximum given in materials acceptance specifications and which is used for verifying the severity of

the test procedure
© ISO 2022 – All rights reserved
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SIST EN ISO 10270:2022
ISO 10270:2022(E)
4 Principle

Specimens of zirconium or its alloys are exposed to high-pressure water or steam at elevated

temperatures for 72 h or 336 h. The corrosion is normally measured by the gain in mass of the

specimens and by the appearance of an oxide film on the specimen surfaces. In some instances, such

as weld evaluation, mass gain measurements are either impractical to make or are not required. When

so specified, the appearance of the specimen is the sole criterion for acceptance. The test pressure in

steam is 10,3 MPa. The tests in water is performed at 18,6 MPa. The pressure is also determined by the

contractor's requirements.
5 Significance

5.1 Specimens are normally tested after careful etching and rinsing. Specimens with as-manufactured

surfaces may also be tested without further surface removal.

5.2 When tubing with a second material clad on the surface is to be tested, the internal cladding is

removed prior to the measurement to avoid erroneous results from differing corrosion behaviour of the

materials.
6 Interference

Autoclave loads that have one or more specimens showing gross oxidation can, by contamination of the

environment, affect results of other specimens in the autoclave.
7 Reagents and materials

During the test, unless otherwise stated, only reagents of recognized analytical grade and only water

as described in 7.4 or 7.5 are used.
7.1 Argon gas, of purity 999,9 ml/l or higher.
7.2 Nitrogen gas, for purging or controlling oxygen content.
7.3 Argon-hydrogen mixture, for purging to remove dissolved oxygen.

7.4 Grade A water, purified water having an electrical resistivity of not less than 1 MΩ·cm at 25 °C as

measured before the start of the test.

7.5 Grade B water, deionized or demineralized water having an electrical resistivity of not less than

0,5 MΩ·cm at 25 °C. Grade A water can be used instead of grade B water.

7.6 Detergents and solvents, for specimen cleaning, including ethanol and acetone.

7.7 Concentrated hydrofluoric acid (HF).
7.8 Concentrated nitric acid (HNO ).
7.9 Concentrated sulfuric acid (H SO ).
2 4
7.10 Control coupon.
7.11 High mass gain coupon.
© ISO 2022 – All rights reserved
---------------------- Page: 14 ----------------------
SIST EN ISO 10270:2022
ISO 10270:2022(E)
8 Apparatus
The apparatus consists of equipment for:
a) etching the specimen when required;

b) measuring the specimens’ surface area and mass, the water resistivity and pH, the test temperature

and pressure, and the etch and rinse temperature;

c) performing the water or steam corrosion tests at elevated temperatures and pressures.

8.1 Etching equipment, comprising an acid bath, a running water rinse and a deionized water rinse

needed for proper metal removal and stain-free rinsing. Polyethylene or polypropylene tanks are

commonly used with a bottom feed for running water rinses. Specimen hangers are generally made

of type 300 series stainless steel. When many specimens are processed, a mechanical dipper for the

etching process is useful.

8.2 Autoclaves, constructed of type 300 series stainless steel or nickel base alloys such as UNS grade

N06600 or N066901. The autoclave is fitted with devices for measurement and control of pressure and

temperature, safety devices and venting valves. Control systems for pressure and temperature are

adequate to meet the requirements of this document. Sample holders and other internal accessories are

also constructed of type 300 or type 400 series stainless steel, or nickel-base alloys such as UNS grade

N06600 or N06690.
8.3 Specimen size measuring equipment, accurate to 50 μm.
8.4 Analytical balance, accurate to 0,1 mg.
9 Hazards

9.1 The chemicals used in preparing specimens for this test are hazardous. Detailed information on

the safe handling of organic compounds, acids and products of zirconium and its alloys are obtained

from competent sources.

9.2 High-temperature, high-pressure autoclave operation is in accordance with the manufacturer's

instructions.

9.3 Hydrogen gas used for the addition to the autoclave steam supply is handled in accordance with

the guidelines for explosives and inflammable substances.

9.4 Cold water is not added directly to the autoclave vessel in order to accelerate cooling upon the

completion of testing.
10 Sampling, test specimens and test units

10.1 The size and the quantity of the test specimens, the method of selection, surface preparation

and test acceptance criteria are specified in the product specification or by agreement between the

purchaser and the seller as stated in the purchase contract. The total surface area for each specimen is

a minimum of 10 cm .
10.2 Each specimen and control coupon is individually identified.

1) UNS grades N06600 and N06690 are examples of suitable products available commercially. This information

is given for the convenience of users of this document and does not constitute an endorsement by ISO of these

products.
© ISO 2022 – All rights reserved
---------------------- Page: 15 ----------------------
SIST EN ISO 10270:2022
ISO 10270:2022(E)
11 Preparation of apparatus

11.1 General requirements for new or reworked autoclaves (8.2) and parts of autoclaves previously

used for testing materials other than in accordance with this document are as follows.

a) Before specimens are tested in a new or reworked autoclave, or in one having new valves, tubing,

gaskets, etc. which are in contact with the test specimen, clean the apparatus thoroughly, wipe

with ethanol or acetone (7.6) and rinse twice with grade B water (7.5).

b) Dry the autoclave or auxiliary equipment by vacuum cleaning, or drain and wipe with a clean,

lint-free cloth and inspect carefully to ensure freedom from contamination. There is no visible

contamination, such as lubricant, residues, dust or dirt, loose oxides or rust, or an oil or grease film

on the water surface, internal surface, gasket or head surfaces.

c) Clean all new and reworked fixtures and jigs to be used in the autoclave and rinse in hot grade B

water.

d) Autoclave the fixtures and jigs for at least 24 h at 400 °C in steam at 10,3 MPa or, preferably, at

360 °C in water at 18,6 MPa.

e) Inspect the parts for corrosion products. If corrosion products are found or electrical resistivity of

the residual water after the test measures less than 0,1 MΩ·cm, clean and autoclave the parts again.

11.2 General requirements for autoclaves and parts in continuous use for corrosion testing in

accordance with this document are as follows.

a) All autoclaves, fixtures, parts and jigs that have been in continuous use and have shown satisfactory

behaviour
...

SLOVENSKI STANDARD
oSIST prEN ISO 10270:2020
01-november-2020

Korozija kovin in zlitin - Preskušanje vodne korozije cirkonijevih zlitin za uporabo

v jedrskih reaktorjih (ISO/DIS 10270:2020)

Corrosion of metals and alloys - Aqueous corrosion testing of zirconium alloys for use in

nuclear power reactors (ISO/DIS 10270:2020)

Korrosion von Metallen und Legierungen - Korrosionsprüfung in wässrigen Lösungen für

in Kernreaktoren angewendete Zirkoniumlegierungen (ISO/DIS 10270:2020)
Corrosion des métaux et alliages - Essais de corrosion aqueuse des alliages de
zirconium utilisés dans les réacteurs nucléaires (ISO/DIS 10270:2020)
Ta slovenski standard je istoveten z: prEN ISO 10270
ICS:
27.120.99 Drugi standardi v zvezi z Other standards related to
jedrsko energijo nuclear energy
77.060 Korozija kovin Corrosion of metals
oSIST prEN ISO 10270:2020 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
oSIST prEN ISO 10270:2020
---------------------- Page: 2 ----------------------
oSIST prEN ISO 10270:2020
DRAFT INTERNATIONAL STANDARD
ISO/DIS 10270
ISO/TC 156 Secretariat: SAC
Voting begins on: Voting terminates on:
2020-09-15 2020-12-08
Corrosion of metals and alloys — Aqueous corrosion
testing of zirconium alloys for use in nuclear power
reactors

Corrosion des métaux et alliages — Essais de corrosion aqueuse des alliages de zirconium utilisés dans les

réacteurs nucléaires
ICS: 77.060; 27.120.10
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Contents Page

Foreword ..........................................................................................................................................................................................................................................v

Introduction ..............................................................................................................................................................................................................................vii

1 Scope (mandatory) ............................................................................................................................................................................................. 1

2 Normative references (mandatory) .................................................................................................................................................. 1

3 Terms and definitions (mandatory) ................................................................................................................................................. 1

4 Principle ........................................................................................................................................................................................................................ 2

5 Significance ................................................................................................................................................................................................................ 2

6 Interference ............................................................................................................................................................................................................... 2

7 Reagents and materials ................................................................................................................................................................................. 2

8 Apparatus ..................................................................................................................................................................................................................... 3

8.1 General ........................................................................................................................................................................................................... 3

9 Hazards ........................................................................................................................................................................................................................... 3

10 Sampling, test specimens and test units ...................................................................................................................................... 4

11 Preparation of apparatus ............................................................................................................................................................................ 4

12 Calibration and standardization .......................................................................................................................................................... 4

12.1 High mass gain coupon preparation ..................................................................................................................................... 4

12.2 Autoclaves ................................................................................................................................................................................................... 4

12.3 Use of control coupons ..................................................................................................................................................................... 5

12.4 Calibration .................................................................................................................................................................................................. 6

13 Conditioning .............................................................................................................................................................................................................. 6

13.1 Test water quality ................................................................................................................................................................................. 6

13.2 Autoclave load restrictions ........................................................................................................................................................... 6

13.3 Test conditions ........................................................................................................................................................................................ 6

13.3.1 Temperature ........................................................................................................................................................................ 6

13.3.2 Pressure ................................................................................................................................................................................... 6

13.3.3 Time ............................................................................................................................................................................................ 6

13.3.4 Tests ............................................................................................................................................................................................ 6

13.4 Specimen preparation ...................................................................................................................................................................... 7

13.4.1 Etched specimens ...................................................................... ...................................................................................... 7

13.4.2 As-manufacturer specimens .................................................................................................................................. 7

14 Procedure..................................................................................................................................................................................................................... 7

14.1 Inspection of specimens ................................................................................................................................................................. 7

14.2 Dimensions, weight and inspection ...................................................................................................................................... 7

14.3 Autoclaving ................................................................................................................................................................................................. 7

14.3.1 Placing of test specimens.......................................................................................................................................... 7

14.3.2 Venting method A ............................................................................................................................................................ 7

14.3.3 Venting method B ............................................................................................................................................................ 8

14.3.4 Closed system method C............................................................................................................................................ 9

14.3.5 Refreshed autoclaving, method D...................................................................................................................... 9

14.4 Post-test measurements and inspection........................................................................................................................... 9

15 Calculation or interpretation of results ....................................................................................................................................10

15.1 Calculation of mass gain...............................................................................................................................................................10

15.2 Visual interpretation of surface appearance ..............................................................................................................10

15.3 Invalid tests .............................................................................................................................................................................................10

16 Test report ................................................................................................................................................................................................................10

Annex A (informative) Guide to specimen preparation .................................................................................................................12

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Bibliography .............................................................................................................................................................................................................................15

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Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following

URL: www .iso .org/ iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 156, Corrosion of metals and alloys.

This second edition cancels and replaces the first edition (ISO 10270:1995), which has been technically

revised.
The main changes compared to the previous edition are as follows:

— Chapter 2 The first paragraph is replaced by “The following documents are referred to in the text

in such a way that some or all of their content constitutes requirements of this document. For

dated references, only the edition cited applies. For undated references, the latest edition of the

referenced document (including any amendments) applies.” And“1990” is replaced by “2012” for the

latest vision of ISO 5814.

— Chapter 3 The title of “ Definitions” is replaced by “Terms and definitions”. And the first paragraph

is replaced by:
“For the purposes of this document, the following terms and definitions apply.
The list below is always included after each option:

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— IEC Electropedia: available at http:// www .electropedia .org/
— ISO Online browsing platform: available at https:// www .iso .org/ obp”.

— Chapter 4 Two sentence are added that “the tests in water shall be performed at 18.6 MPa (2 697

psi)” and”The pressure should also be determined by the contractor requirements” in the end.

— Chapter 5.2 The word of “ internal” is added before “cladding” .

— Chapter 7.1 The words of “ welding grade” is replaced by “purity is 99.99 % or higher”.

— Chapter 7.3 The word of “dissolved” is added before “oxygen”.
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— Chapter 8.1 The bracket is added for the superscript number “1”.

— Chapter 11.1.2 The unit of “1 day” is replaced by “24 h”; and the words of “at 18.6 MPa” is added after

“at 360 °C in water”.
— Chapter 12.1 The word of “Zircalloy” is replaced by “Zircaloy”.

— Chapter 12.3.4 It is added that “However, for product acceptance test, it is better to keep control

coupons as evidence of test effectiveness.” in the end.

— Chapter 14.3.2.1 The tile of “The Relationship between Temperature and the Specific Volumes of

Water” is added for Table 1.

— Annex A.3.1 “3 % (m/m) of hydrofluoric acid (7.7), 39 % (m/m) of nitric acid (7.8)” is instead by

“4 % (m/m) ± 2 % (m/m) of hydrofluoric acid (7.7), 45 % (m/m) ± 5 % (m/m) of nitric acid (7.8)”. And

the sentence is added that “If the different acid ratio is chose to satisfy the requirement of smooth

and shining surface as mentioned in 13.4.1, it is acceptable”in the end.

— Annex A.6 It is added that“ or be placed into the oven, the condition of 60 - 70 °C for one hour is

recommended at the oven ”after “dust and acid fumes”. The sentence is added that “The specimens

need to be cooled to room temperature after removing from the oven” in the end.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
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Introduction

The nuclear industry has been developed in recent years, but the latest standard was published in 1997,

and not revised until now. There are some problems in the standard after 22 years. The revised standard

is more suitable for the application in Nuclear Industry. The revised standard will be more professional

and precise, the customers will understand the standard very well and avoid the misunderstanding.

The problems are :

1) Pressure: There is no pressure in water at 360 °C. In general, saturated vapor pressure of water is

18.6 MPa 360 °C. In the world, the pressure in water at 360 °C is only 18.6 MPa for the corrosion of

zirconium alloys. Many references also prove that the pressure is 18.6 MPa for water at 360 °C. The

pressure shall be added in the text.

2) Re-use: In Chapter 12.3.4, Control coupons may be re-used after mechanical removal of oxide film

followed by etching as described in 13.4.1. Actually, the oxide is very dense and hard to be removed.

The weight gain is not real if metal oxides were still on the surface of the control coupons. To ensure

the experiment effective, it is added that “however, for product acceptance test, it is better to keep

control coupons as evidence of test effectiveness” at the end of the paragraph.

3) Unit: The unit is hour in Chapter 4, but the unit is days in Chapter 13.3.3. Both sentences express

the same meaning, but the unit is different. The unit of hour is applied for the whole text.

4) The range of acid: 3 % (m/m) of hydrofluoric acid and 39 % (m/m) of nitric acid are mentioned in

Appendix 3.1. But 9 % (m/m) ± 1 % (m/m) of hydrofluoric acid, 30 % (m/m) ± 5 % (m/m) nitric

are mentioned in Appendix 3.2. So 4 % (m/m) ± 2 % (m/m) of hydrofluoric acid, 45 % (m/m) ±

5 % (m/m) of nitric acid are chosen for the range of acid bases on the experiments in Appendix 3.1.

5) Dry method: The oven is often applied for drying the samples besides lint-free cloth or dry air. The

oven is more efficiency for the treatment of lots of samples.
Identification of patent holders, if any.
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DRAFT INTERNATIONAL STANDARD ISO/DIS 10270:2020(E)
Corrosion of metals and alloys — Aqueous corrosion
testing of zirconium alloys for use in nuclear power
reactors

WARNING — — This International Standard may involve the use of hazardous materials,

operations and equipment (see clause 9). It is the responsibility of whoever uses this

International Standard to consult and establish appropriate safety and health practices and

determine the applicability of regulatory limitations prior to use.
1 Scope (mandatory)
This International Standard specifies:
a) the determination of mass gain;

b) the surface inspection of products of zirconium and its alloys when corrosion tested in water at

360 °C or in steam at or above 400 °C;
c) that the tests in steam shall be performed at 10.3 MPa (1 500 psi);

This International Standard is applicable to wrought products, castings, powder metallurgy products

and weld metals.

This method has been widely used in the development of new alloys, heat treating practices and for

the evaluation of welding techniques, and should be utilized in its entirety to the extent specified for a

product acceptance test, rather than merely a means of assessing performance in service.

2 Normative references (mandatory)

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

Members of IEC and IS0 maintain registers of currently valid International Standards.

ISO 5813:1983, Water quality — Determination of dissolved oxygen — lodometric method.

ISO 5814:2012, Water quality — Determination of dissolved oxygen — Electrochemical probe method.

3 Terms and definitions (mandatory)
For the purposes of this document, the following terms and definitions apply.
The list below is always included after each option:

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— IEC Electropedia: available at http:// www .electropedia .org/
— ISO Online browsing platform: available at https:// www .iso .org/ obp
3.1
etching
A process for removal of surface metal by action of acids in water.
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3.2
control coupons

Zirconium alloy specimens of known performance used to monitor the validity of the test.

3.3
high mass gain coupons

Zirconium alloy specimens that have been specially heat-treated to produce a mass gain higher than the

maximum given in materials acceptance specifications and which are used for verifying the severity of

the test procedure.
4 Principle

Specimens of zirconium or its alloys are exposed to high-pressure water or steam at elevated

temperatures for 72 h or 336 h. The corrosion is normally measured by the gain in mass of the

specimens and by the appearance of an oxide film on the specimen surfaces. In some instances, such as

weld evaluation, mass gain measurements are either impractical to make or are not required. When so

specified, the appearance of the specimen shall be the sole criterion for acceptance. The test pressure in

steam shall be 10.3 MPa (1 500 psi); the tests in water shall be performed at 18.6 MPa (2 697 psi). The

pressure should also be determined by the contractor requirements.
5 Significance

5.1 Specimens are normally tested after careful etching and rinsing. Specimens with as-manufactured

surfaces may also be tested without further surface removal.

5.2 When tubing with a second material clad on the surface is to be tested, the internal cladding shall

be removed prior to the test.
6 Interference

Autoclave loads that have one or more specimens showing gross oxidation may, by contamination of the

environment, affect results of other specimens in the autoclave.
7 Reagents and materials

During the test, unless otherwise stated, only reagents of recognized analytical grade and only water

as described in 7.4 or 7.5 shall be used.
7.1 Argon gas, purity is 99.99 % or higher.
7.2 Nitrogen gas for purging or controlling oxygen content.
7.3 Argon-hydrogen mixture for purging to remove dissolved oxygen.

7.4 Grade A water — purified water having an electrical resistivity of not less than 1 MΩ cm at 25 °C

as measured before the start of the test.

7.5 Grade B water — deionized or demineralized water having an electrical resistivity of not less than

0.5 MΩ cm at 25 °C. Grade A water can be used instead of grade B water.
7.6 Detergents and solvents for specimen cleaning including ethanol and acetone.
7.7 Concentrated hydrofluoric acid (HF).
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7.8 Concentrated nitric acid (HNO ).
7.9 Concentrated sulfuric acid (H SO ).
2 4
7.10 Control coupons, as defined in 3.2.
7.11 High mass gain coupons, as defined in 3.3.
8 Apparatus
8.1 General
The apparatus shall consist of equipment for:
a) etching the specimens when required;
[1]

b) measuring the specimens surface area and mass, the water resistivity and pH, the test

temperature and pressure, the etch and rinse temperature;

c) perform the water or steam corrosion tests at elevated temperatures and pressures.

8.2 Etching equipment, comprising an acid bath, a running water rinse and a deionized water

rinse needed for proper metal removal and stain-free rinsing. Polyethylene or polypropylene tanks are

commonly used with a bottom feed for running water rinses. Specimen hangers are generally made of

type 300 series stainless steel. When many specimens are processed, a mechanical dipper for the etching

process is useful.

8.3 Autoclaves, constructed of type 300 series stainless steel or nickel base alloys such as UNS grade

NO6600 or NO6690 and manufactured to conform to government regulations governing unfired pressure

vessels. The autoclave is fitted with devices for measurement and control of pressure and temperature,

safety devices and venting valves. Control systems for pressure and temperature shall be adequate to

meet the requirements of this International Standard. Sample holders and other internal accessories are

also constructed of type 300 or type 400 series stainless steel, or nickel-base alloys such as UNS grade

NO6600 or NO6690.
8.4 Specimen size measuring equipment, accurate to 50 μm.
8.5 Analytical balance, accurate to 0.1 mg.
9 Hazards

9.1 The chemicals used in preparing specimens for this test are hazardous. Detailed information on

safe handling of organic compounds, acids and products of zirconium and its alloys should be obtained

from competent sources.

9.2 High-temperature, high-pressure autoclave operation must be in accordance with government

regulations and manufacturer's instructions.

9.3 Hydrogen gas used for addition to the autoclave steam supply must be handled in accordance with

guidelines for explosives and inflammable substances.

9.4 Cold water should not be added directly to the autoclave vessel in order to accelerate cooling upon

the completion of testing.
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10 Sampling, test specimens and test units

10.1 The size and the quantity of the test specimens, the method of selection, surface preparation and

test acceptance criteria shall be specified in the product specification or by agreement between the

purchaser and the seller as stated in the purchase contract. Total surface area for each specimen shall be

a minimum 10 cm .
10.2 Each specimen and control coupon shall be individually identified.
11 Preparation of apparatus

11.1 General requirements for new or reworked autoclaves (8.3) and parts of autoclaves previously

used for testing materials other than in accordance with this International Standard are as follows.

11.1.1 Before specimens are tested in a new or reworked autoclave, or in one having new valves,

tubing, gaskets, etc., which are in contact with the test specimen, clean the apparatus thoroughly, wipe

with ethanol or acetone (7.6), and rinse twice with grade B water (7.5). Dry the autoclave or auxiliary

equipment by vacuum cleaning or drain and wipe with a clean, lint-free cloth and inspect carefully to

ensure freedom from contamination. There should be no visible contamination, such as lubricant,

residues, dust or dirt, loose oxides or rust, or an oil or grease film on the water surface, internal surface,

gasket or head surfaces.

11.1.2 Clean all new and reworked fixtures and jigs to be used in the autoclave and rinse in hot grade

B water. Autoclave the fixtures and jigs for at least 24 h at 400 °C in steam at 10.3 MPa or, preferably, at

360 °C in water at 18.6 MPa. Inspect the parts for corrosion products. If corrosion products are found

or electrical resistivity of the residual water after the test measures less than 0.1 MΩ·cm, clean and

autoclave the parts again.

11.2 General requirements for autoclaves and parts in continuous use for corrosion testing under this

International Standard are as follows. All autoclaves, fixtures, parts and jigs that have been in continuous

use and have shown satisfactory behaviour in prior tests shall be rinsed with grade B water. The fixtures

and jigs for corrosion products shall be inspected after each test and
...

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