Steel — Measurement method for the evaluation of hydrogen embrittlement resistance of high strength steels — Part 1: Constant load test

This document provides a method for the evaluation of the resistance to hydrogen embrittlement (i.e. hydrogen delayed fracture) using constant loading test with hydrogen pre-charged specimens. The amount of hydrogen content absorbed in the specimens is analysed quantitatively by thermal desorption analysis such as gas chromatography, mass spectrometry and so on. In the case of hydrogen continuous charging such as hydrogen absorption in aqueous solution at free corrosion potential, hydrogen absorption in atmospheric corrosion environments and hydrogen absorption in high pressure hydrogen gas, the evaluation method is also briefly described. This method is mainly applicable to the evaluation of hydrogen embrittlement resistance of high strength steel bolts.

Acier — Méthode de mesure pour l'évaluation de la résistance à la fragilisation par l'hydrogène des aciers à haute résistance — Partie 1: Essai de charge constante

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Status
Published
Publication Date
13-Aug-2020
Current Stage
6060 - International Standard published
Start Date
13-Apr-2020
Completion Date
14-Aug-2020
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ISO 16573-1:2020 - Steel -- Measurement method for the evaluation of hydrogen embrittlement resistance of high strength steels
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INTERNATIONAL ISO
STANDARD 16573-1
First edition
2020-08
Steel — Measurement method for the
evaluation of hydrogen embrittlement
resistance of high strength steels —
Part 1:
Constant load test
Acier — Méthode de mesure pour l'évaluation de la résistance à la
fragilisation par l'hydrogène des aciers à haute résistance —
Partie 1: Essai de charge constante
Reference number
ISO 16573-1:2020(E)
ISO 2020
---------------------- Page: 1 ----------------------
ISO 16573-1:2020(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
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CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 16573-1:2020(E)
Contents Page

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

Introduction ..................................................................................................................................................................................................................................v

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

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

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

4 Principle ........................................................................................................................................................................................................................ 1

5 Specimen preparation .................................................................................................................................................................................... 2

6 Hydrogen charging methods .................................................................................................................................................................... 3

6.1 General ........................................................................................................................................................................................................... 3

6.2 Cathodic charge method ................................................................................................................................................................. 3

6.2.1 Hydrogen charging solution ................................................................................................................................... 3

6.2.2 Hydrogen charging conditions ............................................................................................................................. 4

6.3 Hydrogen absorption in aqueous solution at free corrosion potential .................................................. 4

6.4 Hydrogen absorption in atmospheric corrosion environments................................................................... 4

6.5 Hydrogen absorption in high pressure hydrogen gas ........................................................................................... 4

7 Preparation of electroplating solution and electroplating condition ...........................................................5

7.1 General ........................................................................................................................................................................................................... 5

7.2 Electroplating solution ..................................................................................................................................................................... 5

7.3 Electroplating conditions ............................................................................................................................................................... 5

8 Constant loading test........................................................................................................................................................................................ 5

8.1 Constant loading test procedures ........................................................................................................................................... 5

8.2 Presentation of the results ............................................................................................................................................................ 6

9 Post-test specimen treatment ................................................................................................................................................................. 8

10 Hydrogen thermal desorption analysis ........................................................................................................................................ 9

10.1 General ........................................................................................................................................................................................................... 9

10.2 Experimental apparatus (gas chromatograph) .......................................................................................................10

10.3 Experimental apparatus (mass spectrometry) ........................................................................................................10

11 Test report ................................................................................................................................................................................................................10

Bibliography .............................................................................................................................................................................................................................11

© ISO 2020 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 16573-1:2020(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 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 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 17, Steel, Subcommittee SC 7, Methods of

testing (other than mechanical tests and chemical analysis).

This edition cancels and replaces the first edition (ISO 16573:2015), which has been technically revised.

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

— the addition of a note to provide the definition of ρ as the radius of the notch bottom. The definition

of r was unclear and was used in a different way in 2b).

— the temperature in 6.1 and Clause 7 where different, the temperature below −50 °C is used;

— the addition of Figures of unbroken notched specimen and unbroken smooth specimen;

— the addition of research papers in Bibliography.

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.
iv © ISO 2020 – All rights reserved
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ISO 16573-1:2020(E)
Introduction

The mechanical properties of high strength steels, such as tensile strength, elongation and reduction

of area, would be degraded by the effect of hydrogen, known as hydrogen embrittlement, and the

susceptibility of hydrogen embrittlement becomes greater with increasing the strength level of steels.

This document suggests a standardized test method for the evaluation of hydrogen embrittlement

resistance of high strength steels.
© ISO 2020 – All rights reserved v
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INTERNATIONAL STANDARD ISO 16573-1:2020(E)
Steel — Measurement method for the evaluation of
hydrogen embrittlement resistance of high strength
steels —
Part 1:
Constant load test
1 Scope

This document provides a method for the evaluation of the resistance to hydrogen embrittlement

(i.e. hydrogen delayed fracture) using constant loading test with hydrogen pre-charged specimens.

The amount of hydrogen content absorbed in the specimens is analysed quantitatively by thermal

desorption analysis such as gas chromatography, mass spectrometry and so on. In the case of hydrogen

continuous charging such as hydrogen absorption in aqueous solution at free corrosion potential,

hydrogen absorption in atmospheric corrosion environments and hydrogen absorption in high pressure

hydrogen gas, the evaluation method is also briefly described. This method is mainly applicable to the

evaluation of hydrogen embrittlement resistance of high strength steel bolts.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
No terms and definitions are listed in this document.

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 http:// www .electropedia .org/
4 Principle

This test method is used to evaluate material resistance to hydrogen embrittlement. Figure 1 shows

schematic sequences for a) hydrogen pre-charging method and b) hydrogen continuous charging

method. For the hydrogen pre-charging method [see Figure 1 a)], prepare a test specimen which has

a higher hydrogen level by forcibly charging hydrogen into the specimen. Apply constant load to the

hydrogen charged test specimen and measure the time to failure. By testing specimens containing

various contents of diffusible hydrogen, which is mainly responsible for hydrogen embrittlement,

the relationship between diffusible hydrogen content and times to failure can be obtained. Diffusible

hydrogen content can be measured by thermal desorption analysis using the test specimen after failure.

This method can provide at least qualitative comparison of the resistance to hydrogen embrittlement

among several high strength steels having different microstructures or compositions. For the hydrogen

continuous charging method [see Figure 1 b)], a test specimen is loaded in one of the following three

conditions:
a) in aqueous solution at free corrosion potential;
b) in atmospheric corrosion environments;
© ISO 2020 – All rights reserved 1
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ISO 16573-1:2020(E)
c) in high pressure hydrogen gas.

Then, hydrogen analysis is carried out after failure of the specimen. If specimens do not fail within 100 h

(up to 200 h if so formerly agreed), qualitative comparison of the resistance to hydrogen embrittlement

can be made by hydrogen analysis of unbroken specimens.
a) Hydrogen pre-charging method b) Hydrogen continuous charging method
Figure 1 — Flow chart illustrating the test methods
5 Specimen preparation

The dimensions of the specimens shall be in accordance with Figure 2, and other configurations of the

test specimen may be applied. Unless otherwise specified, diameter of the specimen shall be 10 mm.

[2][3]
For samples with smaller diameter (i.e. D = 5 mm), ρ/D = 0,02 may be applied .
2 © ISO 2020 – All rights reserved
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ISO 16573-1:2020(E)
NOTE 1 ρ is radius of the notch bottom.
NOTE 2 Some types of specimen don't have thread.
a) Notched specimen
b) Smooth specimen
Key
d/D 0,6
ρ/D 0,01 or 0,02
Lc/D 7
G/D 5
NOTE 1 ρ is radius of the notch bottom.
NOTE 2 Some types of specimen don't have thread.
Figure 2 — Dimensions and shape of specimens
6 Hydrogen charging methods
6.1 General

There are four hydrogen charging methods, such as cathodic charging, hydrogen absorption in aqueous

solution at free corrosion potential, hydrogen absorption in atmospheric corrosion environments and

hydrogen absorption in high pressure hydrogen gas. The examples of the condition of each method are

as follows.
6.2 Cathodic charge method
6.2.1 Hydrogen charging solution

To estimate the effect of hydrogen on the mechanical properties of steels, the hydrogen is forced to

diffuse into the specimens by the cathodic charging method. For hydrogen pre-charging, the charging

solution should be prepared and the chemical compositions of the solutions are listed in Table 1.

Two kinds of solutions may be used for hydrogen pre-charging. Solution 1 may be used for introducing

a relatively large amount of hydroge
...

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