oSIST prEN ISO 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)

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/DIS 10270:2020)

Korozija kovin in zlitin - Preskušanje vodne korozije cirkonijevih zlitin za uporabo v jedrskih reaktorjih (ISO/DIS 10270:2020)

General Information

• Status: Not Published
• Public Enquiry End Date: 19-Nov-2020
• ICS: 27.120.10 - Reactor engineering
• ICS: 27.120.99 - Other standards related to nuclear energy
• ICS: 77.060 - Corrosion of metals
• Technical Committee: IPKZ - Protection of metals against corrosion
• Current Stage: 5020 - Formal vote (FV) (Adopted Project)
• Start Date: 06-Oct-2021
• Due Date: 24-Nov-2021
• Ref Project: FprEN ISO 10270 - Corrosion of metals and alloys - Aqueous corrosion testing of zirconium alloys for use in nuclear power reactors (ISO/FDIS 10270:2021)

RELATIONS

• Revised: SIST EN ISO 10270:2008 - Corrosion of metals and alloys - Aqueous corrosion testing of zirconium alloys for use in nuclear power reactors (ISO 10270:1995)
• Effective Date: 01-Nov-2020

Standards Content (sample)

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.

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oSIST prEN ISO 10270:2020
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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
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
ISO/CEN PARALLEL PROCESSING
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 10270:2020(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
PROVIDE SUPPORTING DOCUMENTATION. ISO 2020
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oSIST prEN ISO 10270:2020
ISO/DIS 10270:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020

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: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
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oSIST prEN ISO 10270:2020
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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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oSIST prEN ISO 10270:2020
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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.
vi © ISO 2020 – All rights reserved
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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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oSIST prEN ISO 10270:2020
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
...