INTERNATIONAL ISO

STANDARD 15158

First edition
2014-02-15

Corrosion of metals and alloys —

Method of measuring the pitting
potential for stainless steels by
potentiodynamic control in sodium
chloride solution
Corrosion des métaux et alliages — Méthode de mesure du potentiel
iTeh STANDARD
de piqûre des aciersPREVIEW
inoxydables par contrôle potentiodynamique en
solution de chlorure de sodium
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ISO 15158:2014
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Reference number
ISO 15158:2014(E)

© ISO 2014
ISO 15158:2014(E)


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Contents Page

Foreword......................................................................................................................................................................................................................................... iv
Introduction...................................................................................................................................................................................................................................v
1 Scope.................................................................................................................................................................................................................................. 1
2 Principle......................................................................................................................................................................................................................... 1
3 Apparatus...................................................................................................................................................................................................................... 1
3.1 Potentiostat................................................................................................................................................................................................. 1
3.2 Electrode potential-measuring instrument.................................................................................................................... 1
3.3 Current-measuring instruments............................................................................................................................................... 1
3.4 Specimen holder..................................................................................................................................................................................... 2
3.5 Test cell........................................................................................................................................................................................................... 2
3.6 Auxiliary electrode............................................................................................................................................................................... 2
3.7 Reference electrode............................................................................................................................................................................. 2
4 Specimens..................................................................................................................................................................................................................... 3
5 Procedure..................................................................................................................................................................................................................... 3
5.1 Preparation of reference electrodes...................................................................................................................................... 3
5.2 Preparation of specimen................................................................................................................................................................. 3
5.3 Preparation of solution..................................................................................................................................................................... 3
5.4 Setting up test........................................................................................................................................................................................... 4
5.5 Recording...................................................................................................................................................................................................... 4
5.6 iTeh STANDARD PREVIEW
Ending test................................................................................................................................................................................................... 5
6 (standards.iteh.ai)
Statistical analysis of pitting potential data.............................................................................................................................. 5
7 Test report.................................................................................................................................................................................................................... 5
ISO 15158:2014
Annex A (informative) Specimen holder........................................................................................................................................................... 7
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Annex B (informative) An example6dc7c7440536/iso-15158-2014 of statistical analysis of pitting potential data..........................................11
Bibliography.............................................................................................................................................................................................................................. 13

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ISO 15158:2014(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
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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
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to Trade (TBT) see the following URL: Foreword - Supplementary information
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The committee responsible for this document is ISO/TC 156, Corrosion of metals and alloys.
ISO 15158:2014
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Introduction
Although stainless steel is generally used as a corrosion-resistant material, it is susceptible to pitting
corrosion, crevice corrosion, stress corrosion cracking, etc. Among those, pitting corrosion is one of
the most common phenomena that occur on stainless steels. A commonly used parameter to evaluate
the pitting corrosion resistance of stainless steel, is so-called pitting potential that defines the lowest
potential below which stables pits are not considered to grow. Since pitting corrosion generally shows
a stochastic nature dependent upon inhomogeneity in terms of size, orientation, alloying components,
impurity, inclusions, segregation, surface treatment, history, elapsed time, fluctuation of environment,
etc., its measurement requires at least a couple of values.

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INTERNATIONAL STANDARD ISO 15158:2014(E)

Corrosion of metals and alloys — Method of measuring the

pitting potential for stainless steels by potentiodynamic
control in sodium chloride solution

1 Scope
This International Standard describes the procedure for determining the pitting potential for stainless
steels (austenitic, ferritic/austenitic, ferritic, martensitic stainless steel) under potentiodynamic control.
The principal advantage compared with other potentiostatic test methods[1][2] is the rapidity of this test
method, with which the pitting potential can be measured in a single potential scan.
The pitting potential as determined by this International Standard can be used as a relative index of
performance. For example, one can compare the relative performances for different lots of stainless-
steel grades and products. The test described in this International Standard is not intended to determine
the pitting potential at which actual pitting can occur under real service conditions, or not.

2 Principle
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The test involves increasing the anodic potential of the specimen at a specified scan rate while exposing
the specimen to a normalized sodium chloride solution at a constant temperature.
(standards.iteh.ai)
The pitting potential (V’c10 or V’c100) (see JIS G 0577 ) is defined as the potential at which the current
[3]
density exceeds 10 μA/cm2 or 100 μA/cm 2 for
ISO more than 60 s. A 60 s delay is used in order to ensure
15158:2014
that the observed current increase originates from stably propagating pitting, since short-lived current
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peaks originate from metastable pitting. 6dc7c7440536/iso-15158-2014
The specimen holder and the specimen itself are designed to ensure that crevice corrosion does not
occur.

3 Apparatus

3.1 Potentiostat
The potentiostat shall be capable of controlling the electrode potential to within ±1 mV of a preset value.

3.2 Electrode potential-measuring instrument

The instrument shall have high input impedance sufficient to eliminate potential read error due to
current drawn by the instrument during measurement; impedance of the order of 1011 Ω to 1014 Ω is
typical. The sensitivity and accuracy of the instrument should be sufficient to detect a change of 1,0 mV.

3.3 Current-measuring instruments

The current in the circuit is evaluated from the potential drop measured across a known resistor. In many
potentiostats, this measurement is made internally. But measurements may also be made externally by
locating a resistor in the current line from the auxiliary electrode to the auxiliary connection of the
potentiostat. The instrument shall be capable of measuring a current within 2 % error around the actual
value.

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ISO 15158:2014(E)


3.4 Specimen holder

3.4.1 Any part of the specimen holder coming into contact with the test solution shall be made of an
inert material.

3.4.2 The specimen holder shall be designed to ensure that crevice corrosion does not occur at the
contact area between the specimen holder and the specimen. Some methods to prevent such crevice
attack, using a flushed port cell, or using a flushed specimen holder, are outlined in A.1 and A.2.

3.4.3 If the specimen holder avoiding crevice corrosion cannot be used, the specimen electrode could
be treated by the special method as outlined in A.3.

3.5 Test cell

3.5.1 The test cell shall contain the test specimen, a Luggin capillary probe connected to an external
reference electrode for measuring the electrode potential, an auxiliary electrode, a port for insertion of a
temperature measuring device, a bubbler for de-aeration by inert gas such as N2 or Ar, and/or a facility
for stirring the solution in a repeatable manner.
NOTE This can be achieved by using a mechanical stirring device, or simply by bubbling inert gas through the
solution at a controlled rate.

An accuracy of the temperature measuring instrument shall be ±0,4 °C.

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3.5.2 A double-walled cell is commonly used to enable the solution to be cooled or to be heated by
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recirculating a liquid from an external cooling or heating bath to the outer chamber of the cell.

3.5.3 The tip of the Luggin capillary probe shall be ISOpositioned

15158:2014 so that it is at a distance from the specimen
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of about, but not closer than, twice the diameter of the tip.
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3.5.4 Any part of the test cell or specimen holder that comes into contact with the solution shall be
constructed from an inert material. Polycarbonate, glass and polytetrafluoroethylene (PTFE) are suitable
materials.

3.5.5 The ratio of the volume of solution in the test cell to the specimen area shall be at least 100 ml/cm2.

3.6 Auxiliary electrode

The auxiliary electrode is commonly prepared from high purity platinum. Other materials may be used
provided they are inert. The auxiliary electrode may be constructed in the form of sheet, rod, wire, or
in the form of gauze supported on a glass frame. The area of the auxiliary electrode shall be at least the
area of the specimen.
Graphite may be used as an auxiliary electrode, but care shall be taken to avoid contamination; desorption
of species retained in the graphite may be necessary prior to usage.

3.7 Reference electrode

3.7.1 The reference electrode shall be maintained at ambient temperature external to the test cell, and
shall be connected to the test cell via a Luggin capillary probe.

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3.7.2 Commonly used electrode is the saturated silver/silver chloride electrode (sat.SSCE). The
potentials of these electrodes relative to the standard hydrogen electrode at 25 °C are given in ISO 17474.
[4]

If the saturated calomel electrode (SCE) is used, strict control to handle mercury and mercury containing
substances in terms of health and environmental issues shall be taken. The use of saturated calomel
electrode shall follow nation’s rules and regulations.

4 Specimens

4.1 The specimen shall be taken from a test material such that the test area is minimum 1,0 cm2.
Different surfaces are permitted, if they are used in actual application: e.g. different heat treatments, and
different surface finish.

4.2 The specimen may be taken by sawing, cutting, grinding, etc. The depth affected by machining shall
be removed by progressive grinding so that the traces of machining may not affect the test results.
NOTE If relevant parties agree, any surface finishes different from the above recommendation may apply as
far as they are reproducible.

5 Procedure

5.1 Preparation of reference electrodes

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5.1.1 (standards.iteh.ai)
The difference in potential among the reference electrode and two other validation electrodes
shall be measured. The latter electrodes shall be traceable to the standard hydrogen electrode, and shall
be maintained solely for the purpose of validation. If the potential is different by greater than 3 mV, the
ISO 15158:2014
electrode shall be rejected.
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5.1.2 The validation electrodes shall be stored in optimum conditions and regularly compared. If the
potential difference between these varies by more than 1 mV, replacement shall be undertaken.

5.2 Preparation of specimen

5.2.1 The final grinding of the specimen may be dry or wet. Before measurement, the specimen is
recommended to be ground with 600 grit paper, and shall then be thoroughly cleaned.
NOTE 1 After grinding, it takes time for the air formed film to achieve a quasi-steady condition. The most rapid
change in filming occurs in the first period with progressive stabilization at longer periods.

NOTE 2 A minimum time period of 24 h is recommended. However, a shorter period may be adopted depending
on the purpose of the test. Nevertheless, the time period in a set of tests should be consistent.

NOTE 3 If relevant parties agree, surface finishes different from the above recommendation may apply as far
as they are reproducible.

5.2.2 The specimen shall be cleaned prior to immersion into the test solution, by degreasing, rinsing in
high purity water (with a conductivity less than 1 μS/cm), followed by ethanol or a similar solvent, and
then air drying. After degreasing, care shall be taken not to contaminate the test surface of the specimen.

5.3 Preparation of solution

5.3.1 The solution shall be prepared using reagent-grade chemicals and high purity water.

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5.3.2 The test solution should reflect the intended application; otherwise 1 M (k mol m−3) sodium
chloride aqueous solution may be used.
NOTE The recommended test solution of 1 M sodium chloride aqueous solution can be prepared by dissolving
58,44 g of reagent-grade sodium chloride into 1 000 mL of distilled or ion-exchange water.

5.4 Setting up test

5.4.1 The exposed surface area of the test specimen shall be measured.

5.4.2 The standard temperature of the test solution shall be (30 ± 1) °C.

The tests may be performed at a different temperature depending on the purpose, but the same
temperature for a particular set of tests shall be applied.

5.4.3 For anodic polarization, completely immerse the test surface area in the de-aerated test solution;
leave it to stand there to stabilize temperature and corrosion potential for at least 1 min. Then, start
potential sweeping at the rate of 10 mV/min from corrosion potential until the anodic current density
reaches more than 500 µA/cm2 and less than 1 000 µA/cm2. In case statistical analysis of the potential
data was intended, the sweep rate of 20 mV/min may be used. If these sweep rates are not available by
reason of the apparatus or other, a sweep rate close to it may be used.

Regardless of the type of test assembly (see Annex A), deaeration of the solution shall be undertaken
prior to immersion. A deaeration period of 1 h per litre of test solution is usually sufficient at typical gas
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5.4.4
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The pitting potential shall be expressed by the value of the potential for which pitting becomes
stable; i.e. current density increases continuously with potential as shown in Figure 1. The pitting potential
ISO 15158:2014
is defined as the potential corresponding to the anodic current density of 10 µA/cm2 or 100 µA/cm2 of
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the stable pitting region. The pitting potentials shall be denoted as V’C10 or V’C100, respectively. Figure 1
6dc7c7440536/iso-15158-2014
shows an example of the measurement.

5.4.5 For each test, use a fresh specimen and a fresh test solution.

5.5 Recording
The value of pitting potential measurement shall be recorded in volts (V), down to three decimal places.
Also, the sweep rate and grinding condition prior to the test, the reference electrode, time elapsed
between grinding and immersion, and the test temperature shall be noted (see Clause 7).

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Figure 1 — Example of anodic polarization curve of 4301-304-00-I stainless steel at 30 °C with

respect to potential E and current density i, where the test was performed in deaerated 1 M
NaCl solution with sweep rate of 10 mV/min, just after dry grinding followed by cleaning

5.6 Ending test

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5.6.1 The test shall be terminated when the pitting potential has been determined.
ISO 15158:2014
5.6.2 The specimen shall be removed from the solution and rinsed in water, cleaned with ethanol,
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rinsed with high purity water, cleaned 6dc7c7440536/iso-15158-2014
with ethanol or a similar solvent, and dried in air.

5.6.3 Using a magnifier with a capacity of 20 times or more, observation of the measured specimen
shall be conducted, to confirm the pitting occurred, and to ensure any crevice corrosion had not occurred.
If corroded crevice is found, exclude this test from the results.

6 Statistical analysis of pitting potential data

6.1 Pitting corrosion of stainless steels shows statistical nature, thus the number of experiments for a
given condition should be considered among relevant parties to obtain the reliable average and standard
deviation values. At least two experiments for a condition are required for statistical analysis. Since the
total area of the specimen is one of factors in determining the probability of finding the weakest site,
the number of repeats should reflect the specimen area. For the 1 cm2 area as recommended in this
International Standard, five repeats or more are recommended.

6.2 The average value of pitting potential data shall be calculated. To show results for a condition, an
example of statistical analysis of pitting potentials is shown in Annex B. For more details on statistical
analyses, the literature[5] in the Bibliography can be consulted.

7 Test report
The test report shall include the following information:
a) reference to this International Standard, i.e. ISO 15158:2014;

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