BS ISO 16573:2015

BSI Standards Publication

Steel — Measurement method

for the evaluation of hydrogen
embrittlement resistance of
high strength steels
BS ISO 16573:2015 BRITISH STANDARD

National foreword
This British Standard is the UK implementation of ISO 16573:2015.
The UK participation in its preparation was entrusted to Technical
Committee ISE/101/7, Methods of physical and metallographic
testing.
A list of organizations represented on this committee can be
obtained on request to its secretary.
This publication does not purport to include all the necessary
provisions of a contract. Users are responsible for its correct
application.
© The British Standards Institution 2015.
Published by BSI Standards Limited 2015
ISBN 978 0 580 79650 0
ICS 77.040.99
Compliance with a British Standard cannot confer immunity from
legal obligations.
This British Standard was published under the authority of the
Standards Policy and Strategy Committee on 30 April 2015.
Amendments/corrigenda issued since publication
Date Text affected
 BS ISO 16573:2015

INTERNATIONAL ISO
STANDARD 16573

First edition
2015-04-01

Steel — Measurement method for the

evaluation of hydrogen embrittlement
resistance of high strength steels
Acier — Méthode de mesure pour l’évaluation de la résistance à la
fragilisation par l’hydrogène des aciers à haute résistance

Reference number
ISO 16573:2015(E)

© ISO 2015
BS ISO 16573:2015
ISO 16573:2015(E)


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 BS ISO 16573:2015
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Contents Page

Foreword......................................................................................................................................................................................................................................... iv
Introduction...................................................................................................................................................................................................................................v
1 Scope.................................................................................................................................................................................................................................. 1
2 Principle......................................................................................................................................................................................................................... 1
3 Specimen preparation..................................................................................................................................................................................... 3
4 Hydrogen charging methods..................................................................................................................................................................... 3
4.1 General............................................................................................................................................................................................................ 3
4.2 Cathodic charge method.................................................................................................................................................................. 3
4.2.1 Hydrogen charging solution.................................................................................................................................... 3
4.2.2 Hydrogen charging conditions.............................................................................................................................. 4
4.3 Hydrogen absorption in aqueous solution at free corrosion potential................................................... 4
4.4 Hydrogen absorption in atmospheric corrosion environments................................................................... 4
4.5 Hydrogen absorption in high pressure hydrogen gas............................................................................................ 4
5 Preparation of electroplating solution and electroplating condition............................................................ 5
5.1 General............................................................................................................................................................................................................ 5
5.2 Electroplating solution...................................................................................................................................................................... 5
5.3 Electroplating conditions................................................................................................................................................................ 5
6 Constant loading test........................................................................................................................................................................................ 5
6.1 Constant loading test procedures............................................................................................................................................ 5
6.2 Presentation of the results............................................................................................................................................................. 6
7 Post-test specimen treatment.................................................................................................................................................................. 8
8 Hydrogen thermal desorption analysis......................................................................................................................................... 8
8.1 General............................................................................................................................................................................................................ 8
8.2 Experimental apparatus (gas chromatograph)........................................................................................................... 8
8.3 Experimental apparatus (mass spectrometry)............................................................................................................ 9
9 Test report.................................................................................................................................................................................................................... 9
Bibliography.............................................................................................................................................................................................................................. 10

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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
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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
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to Trade (TBT), see the following URL: Foreword — Supplementary information.
The committee responsible for this document is ISO/TC 17, Steel, Subcommittee SC 7, Methods of testing
(other than mechanical tests and chemical analysis).

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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 International Standard suggests a standardized test method for the evaluation of hydrogen
embrittlement resistance of high strength steels.

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BS ISO 16573:2015
 BS ISO 16573:2015
INTERNATIONAL STANDARD ISO 16573:2015(E)

Steel — Measurement method for the evaluation of

hydrogen embrittlement resistance of high strength steels
WARNING — Persons using this International Standard should be familiar with normal laboratory
practice. This International Standard does not purport to address all of the safety problems, if
any, associated with its use. It is the responsibility of the user to establish appropriate safety and
health practices and to ensure compliance with any national regulatory conditions.

1 Scope
This International Standard 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 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;
c) in high pressure hydrogen gas.

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Then, hydrogen analysis is carried out after failure of the specimen. If specimens do not fail up to 100 h
(up to 200 h, if necessary), 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

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3 Specimen preparation
The dimensions of the specimens are shown in Figure 2, and other configurations of the test specimen
may be applied. It is recommended to use specimens of 10 mm in diameter as a standard size. For samples
with smaller diameter (i.e. D = 5 mm), r/D = 0,02 may be applied.[1][2]

a)  Notched specimen

b)  Smooth specimen

d/D 0,6
r/D 0,01 or 0,02
Lc/D 7
G/D 5

Figure 2 — Dimensions and shape of specimens

4 Hydrogen charging methods

4.1 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.

4.2 Cathodic charge method

4.2.1 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 hydrogen to the specimens and Solution 2 may be used for introducing a small
amount of hydrogen.

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Table 1 — Chemical composition of the solutions for hydrogen charging

Content
Charging solution Element Mark
g /L
NaCl 30
Solution 1 Large amount of hydrogen
NH4SCN 3
Solution 2 NaOH 4 Small amount of hydrogen

4.2.2 Hydrogen charging conditions

The electro-chemical cell for hydrogen pre-charging may be placed in a 200 ml to 1 000 ml beaker. It
is recommended that the anode of the electrochemical cell be made of platinum wire of spiral type
of 0,5 mm in diameter and 2 m in length (counter electrode), and the specimen works as the cathode
(working electrode). After the Pt wire and the specimen are placed in the cell, apply the constant current
of its current density in the range of 0 A/m2 ~20 A/m2 by using potentio/galvanostat for 48 h. A charging
time of 48 h is recommended, but other charging times are also optional as long as a total time of 72 h is
reached for hydrogen charging and the homogenization treatment by room temperature exposure after
cadmium (Cd) plating. For materials with low hydrogen diffusion coefficient, the hydrogen charging
time and the total time may be increased. The specimen’s surface area should be calculated for proper
current supply. The pre-charged hydrogen amount may be changed by varying the current density or
pre-charging time. However, it is recommended to use fixed pre-charging time and current density to
get reproducible test results.

4.3 Hydrogen absorption in aqueous solution at free corrosion potential

For hydrogen charging by corrosion in acid, HCl solutions or HCl with CH3COOH/CH3COONa buffered
solutions are often used. For example, specimen shall be immersed in 5 % HCl solution at room
temperature. Immersion time shall be determined based on the specimen size and hydrogen diffusion
coefficient of the tested material.

4.4 Hydrogen absorption in atmospheric corrosion environments

For hydrogen charging by atmospheric corrosion, the salt spray test (SST) or cyclic corrosion tests (CCT)
including salt spraying, drying and humidifying are carried out. As an example, desirable CCT processes
are listed in Table 2.

Table 2 — Example of CCT processes

Process Conditions Time

Salt spray 5 % NaCl, 35 °C 2h
Dry 20 % to 30 % humidity, 60 °C 4h
Wet ≥95 % humidity, 50 °C 2h

4.5 Hydrogen absorption in high pressure hydrogen gas

For hydrogen charging by hydrogen gas, the specimens shall be exposed directly to gaseous hydrogen
up to 140 MPa at above room temperature. Exposure time shall be determined based on the specimen
size and hydrogen diffusion coefficient of the tested material. However, extreme care is necessary and it
is not recommended due to the danger of experiment.

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5 Preparation of electroplating solution and electroplating condition

5.1 General
The plating process is applied for the hydrogen pre-charging method in order to prevent hydrogen
release during the loading test.

5.2 Electroplating solution

After hydrogen pre-charging, Cd plating should be conducted to prevent the release of hydrogen from the
specimens during constant loading test. Cd is a well-known toxic material but the hydrogen diffusivity in
Cd is known to be nearly zero. Instead of using toxic Cd, other appropriate plating materials, for example
Zn, may be applied. The elements for Cd plating solution and the amounts of each element are listed in
Table 3. The pH of the solution should be 3 pH to 5 pH. To adjust the pH of the solution, one can add H3BO4
or ammonium solution. (Please make reference to the recommended Zn plating solution in Table 3).

Table 3 — Elements for Cd and Zn plating solutions and the amounts of each element

Solution Element Type Amount

Cd(BF4)2 solution [(C) = 50 %] 427 g
NH4BF4 solute 48 g
Cd plating solution H3BO4 solute 21,6 g
H2O (distilled) solvent 460 ml
pH - 3 to 5
ZnCl2 solute 45 g
KCl solute 234 g
H3BO4 solute 21,6 g
Zn plating solution
Sodium Dodecyl Sulfate solute 0,5 g
H2O (distilled) solvent 700 ml
pH - 5 to 6

5.3 Electroplating conditions

An electrochemical reaction is used for Cd plating. Immerse the metal platinum (Pt) anode into the
prepared Cd solution, and immerse the specimen in order for it to work as a cathode. After hydrogen
pre-charging, clean the specimens by mechanical grinding (polishing) or with 0,1 N HCl and 0,1 N NaOH
by ultrasonic cleaner for 30 s, respectively. Then, immerse the specimens in Cd plating solution and
apply a constant current of 0,5A for 300 s. Other conditions of current and time may also be used for Cd
plating. Using the potential difference, Cd is adhered to the surface of the specimen.
The thickness of Cd plating should be at least 15 μm or higher to prevent hydrogen release. Extreme care
is needed to handle the solutions containing Cd during the entire Cd plating procedures.

6 Constant loading test

6.1 Constant loading test procedures

The suggested methods for the constant loading test are the following.
a) Use adequate jig to apply uniaxial loading to the specimens.

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b) Specimens containing various diffusible hydrogen content should be used to measure the time to
failure. In the case of hydrogen continuous charging, various current densities should be applied to
measure the time to failure of a specimen.
c) Stress ratio (applied stress/tensile stress) should be in the range of between 0,3 and 0,9.
NOTE Tensile strength is measured in evaluated type of specimen without hydrogen charge in advance.

d) If the specimens are not fractured after up to 100 h (up to 200 h, if necessary), one can conclude that
these specimens do not fracture under these conditions and discontinue the test.
e) To ensure recurrence, it is recommended that at least three specimens be tested at the same stress ratio.
f) After the constant loading test, diffusible hydrogen contents of the specimen should be immediately
measured. If it is impossible to measure diffusible hydrogen content immediately following the
test, specimens shall be preserved below –30 °C, preferably in liquid nitrogen, to prevent hydrogen
release from the fractured surface.

6.2 Presentation of the results

a) Figure 3 shows an example of the results of the constant loading test.
b) The abscissa indicates the time-to-failure of the specimens and the ordinate represents the diffusible
hydrogen content or the applied stress ratio (applied stress/notch tensile stress).
c) The critical hydrogen content below which the fracture does not occur is defined as the amount of
hydrogen of the specimen which is not fractured up to 100 h (see Figure 3).
d) It may be concluded that the susceptibility to hydrogen embrittlement is greater if time-to failure is
shorter when tested at the same stress ratio and comparable hydrogen content.
As an additional evaluation method, local hydrogen concentration and local stress may be calculated by
numerical method for comparing the results of specimens with different stress concentration factors.[3]

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Key
X time to failure, h
Y diffusible hydrogen content, % (mass fraction or mass ppma)
a   0,01 % (volume fraction) is the equivalent of 100 ppm; ppm is a deprecated unit.
FP16T and TM16T denote full pearlite microstructure and tempered martensite microstructure, respectively,
having the same tensile strength of 1 600 MPa.[4]

Figure 3 — Example of the results of the constant loading test (time to failure vs diffusible
hydrogen content)

Key
X time to failure, h
Y stress ratio, σap/σnb
Stress ratio (σap/σnb) represents applied stress/notch tensile stress.

Figure 4 — Example of the results of the constant loading test

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7 Post-test specimen treatment

After specimens are fractured, the following process shall be applied.
a) Keep fractured specimens in liquid nitrogen to prevent hydrogen desorption.
b) Cut fractured specimens for the hydrogen analysis from the nearest point to the fractured surface
toward the thread (see Figure 5).
Dimensions in millimetres

a)  Notched specimen

b)  Smooth specimen

The shaded area represents the part taken for hydrogen content analysis.

Figure 5 — Hydrogen content analysis

c) For the Cd-coated specimens (pre-charged condition), removing the Cd layer is necessary before
analysing diffusible hydrogen content. To remove the Cd layer, the cut specimen is immersed into Cd
plating solution and the electrodes are connected in a reverse way of the Cd plating, i.e. the anode is
the specimen and the cathode is the platinum (Pt). A constant current of 1,2 A is applied for 5 min to
remove the Cd layer completely. After the electrochemical process, the specimens should be cleaned
with ethanol by ultrasonic cleaner for 30 s. After removing the Cd layer, the specimen shall be kept
in liquid nitrogen again before performing hydrogen thermal desorption analysis. (Removing the
Zn layer is same as removing the Cd layer.) This procedure should not be applied for the continuous
charging method.

8 Hydrogen thermal desorption analysis

8.1 General
In general, diffusible hydrogen is calculated by integrating the first peak of the curve of thermal
desorption analysis. When several peaks are observed at low temperature (i.e. below 400 °C), diffusible
hydrogen may be calculated by integrating peaks below 400 °C of the curve of thermal desorption
analysis. Since the heating rate does not have a significant influence on test results, high heating rate
such as 100 °C/h is recommended. The heating rate should be reported.

8.2 Experimental apparatus (gas chromatograph)

The equipment for thermal desorption analysis consists of 3 parts: heating, gas sampling, and detecting.
When the specimens are heated, hydrogen inside of the specimens diffuses out and flows into the gas
chromatography column with carrier gas (high purity Ar or He gas). The heating rate is fixed at 100 °C/h

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and the specimen is heated up to 400 °C. Gases can be separated by an adsorption column. For the
accurate measurement of hydrogen content, measuring the background is recommended.

8.3 Experimental apparatus (mass spectrometry)

When applying radio frequency voltage, only selected gas or ion is detected due to its characteristic
mass-to-charge ratio. Hydrogen can be detected continuously during heating. The heating rate is fixed
at 100 °C/h and the specimen is heated up to 400 °C.

9 Test report
The test report shall contain at least the following information unless otherwise agreed by the
parties concerned:
a) a reference to this International Standard, i.e. ISO 16573;
b) information about the sample (i.e. chemical composition, heat treatment);
c) the type of specimen (dimensions and shape);
d) the mechanical properties of the specimen (i.e. yield strength, tensile strength, notch tensile
strength, elongation);
e) the method and condition of hydrogen pre-charging (i.e. current density, charging solution,
charging time);
f) the constant loading test results (i.e. diffusible hydrogen content vs. time-to-failure at the specific
stress ratio, stress ratio vs. time-to-failure);
g) the method of hydrogen thermal desorption analysis (the type of detector of hydrogen, heating rate);
h) any deviation(s) from recommendations written in the text (for example, electro plating condition);
i) the reference number of the report and the date;
j) the name of the analyst(s).

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Bibliography

[1] Yamasaki S. Evaluation Method for Delayed Fracture Susceptibility of Steels and Development
of High Tensile Strength Steels with High Delayed Fracture Resistance, Nippon Steel Technical
Report, No. 80. July 1999, pp. 50–55
[2] Takagi S. Parameters for the Evaluation of Hydrogen Embrittlement of High Strength Steel.
Tetsu-to-Hagane. 2000, 86, pp. 689–695
[3] Wang M. Determination of the critical hydrogen concentration for delayed fracture of high strength
steel by constant load test and numerical calculation. Corros. Sci. 2006, 48, pp. 2189–2202
[4] Kim J.S. Microstructural Influences on Hydrogen Delayed Fracture of High Strength Steels.
Mater. Sci. Eng. A. 2009, 505, pp. 105–110

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