This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: A262 − 15 (Reapproved 2021)

Standard Practices for

Detecting Susceptibility to Intergranular Attack in Austenitic
Stainless Steels1
This standard is issued under the fixed designation A262; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope based on visual examination of bend specimens and, therefore,

1.1 These practices cover the following five tests: classifies the specimens only as acceptable or nonacceptable.
1.1.1 Practice A—Oxalic Acid Etch Test for Classification 1.4 The presence or absence of intergranular attack in these
of Etch Structures of Austenitic Stainless Steels (Sections 4 to tests is not necessarily a measure of the performance of the
13, inclusive), material in other corrosive environments. These tests do not
1.1.2 Practice B—Ferric Sulfate-Sulfuric Acid Test for De- provide a basis for predicting resistance to forms of corrosion
tecting Susceptibility to Intergranular Attack in Austenitic other than intergranular, such as general corrosion, pitting, or
Stainless Steels (Sections 14 to 25, inclusive), stress-corrosion cracking.
1.1.3 Practice C—Nitric Acid Test for Detecting Suscepti- NOTE 1—See Appendix X1 for information regarding test selection.
bility to Intergranular Attack in Austenitic Stainless Steels
(Sections 26 to 36, inclusive), 1.5 The values stated in SI units are to be regarded as
1.1.4 Practice E—Copper–Copper Sulfate–Sulfuric Acid standard. The inch-pound equivalents are in parentheses and
Test for Detecting Susceptibility to Intergranular Attack in may be approximate.
Austenitic Stainless Steels (Sections 37 to 46, inclusive), and 1.6 This standard does not purport to address all of the
1.1.5 Practice F—Copper–Copper Sulfate–50 % Sulfuric safety concerns, if any, associated with its use. It is the
Acid Test for Detecting Susceptibility to Intergranular Attack responsibility of the user of this standard to establish appro-
in Molybdenum-Bearing Austenitic Stainless Steels (Sections priate safety, health, and environmental practices and deter-
47 to 58, inclusive). mine the applicability of regulatory limitations prior to use.
Some specific hazards statements are given in 10.1, 20.1.1,
1.2 The Oxalic Acid Etch Test is a rapid method of
20.1.9, 31.3, 34.4, 53.1.1, and 53.1.10.
identifying, by simple etching, those specimens of certain
1.7 This international standard was developed in accor-
stainless steel grades that are essentially free of susceptibility
dance with internationally recognized principles on standard-
to intergranular attack associated with chromium carbide
ization established in the Decision on Principles for the
precipitates. These specimens will have low corrosion rates in
Development of International Standards, Guides and Recom-
certain corrosion tests and therefore can be eliminated
mendations issued by the World Trade Organization Technical
(screened) from testing as “acceptable.” The etch test is
Barriers to Trade (TBT) Committee.
applicable only to those grades listed in the individual hot acid
tests and classifies the specimens either as “acceptable” or as
“suspect.” 2. Referenced Documents
2.1 ASTM Standards:2
1.3 The ferric sulfate-sulfuric acid test, the copper–copper
A370 Test Methods and Definitions for Mechanical Testing
sulfate–50 % sulfuric acid test, and the nitric acid test are based
of Steel Products
on weight loss determinations and, thus, provide a quantitative
A380/A380M Practice for Cleaning, Descaling, and Passi-
measure of the relative performance of specimens evaluated. In
vation of Stainless Steel Parts, Equipment, and Systems
contrast, the copper–copper sulfate–16 % sulfuric acid test is
D1193 Specification for Reagent Water
E3 Guide for Preparation of Metallographic Specimens
1
These practices are under the jurisdiction of ASTM Committee A01 on Steel,
Stainless Steel and Related Alloys and are the direct responsibility of Subcommittee
2
A01.14 on Methods of Corrosion Testing. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Sept. 1, 2021. Published September 2021. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1943. Last previous edition approved in 2015 as A262 – 15. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/A0262-15R21. the ASTM website.

*A Summary of Changes section appears at the end of this standard

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

1
 A262 − 15 (2021)
2.2 ASME Code:3 E—Copper-Copper Sulfate–16 % Sulfuric Acid Test, and Prac-
BPVC ASME Boiler and Pressure Vessel Code, Section IX tice F—Copper-Copper Sulfate–50 % Sulfuric Acid Test.
2.3 ACS Specifications:4 4.4 Each of these other practices contains a table showing
ACS Reagent Chemicals Specifications and Procedures which classifications of etch structures on a given stainless
2.4 ISO Standard:5 steel grade are equivalent to acceptable or suspect performance
ISO 3651-2 Determination of resistance to intergranular in that particular test. Specimens having acceptable etch
corrosion of stainless steels — Part 2: Ferritic, austenitic structures need not be subjected to the hot acid test. Specimens
and ferritic-austenitic (duplex) stainless steels — Corro- having suspect etch structures must be tested in the specified
sion test in media containing sulfuric acid hot acid solution.
3. Purity of Reagents 4.5 There are two classes of specimens to be considered:
base metal, and process-affected metal.
3.1 Purity of Reagents—Reagent grade chemicals shall be
4.5.1 Process-affected metal contains any condition that
used in all tests. Unless otherwise indicated, it is intended that
affects the corrosion properties of the material in a non-uniform
all reagents conform to the specifications of the Committee on
way, such as (but not limited to) welds; carburized. nitrided, or
Analytical Reagents of the American Chemical Society6 where
oxidized surfaces; mechanical deformation; and areas affected
such specifications are available. Other grades may be used,
by heat. Base metal has none of these conditions.
provided it is first ascertained that the reagent is of sufficiently
4.5.2 Because Practices B, C, and F involve immersing the
high purity to permit its use without lessening the accuracy of
entire specimen and averaging the mass loss over the total
the test result.
specimen area, and because welding, carburization, mechanical
3.2 Purity of Water—Unless otherwise indicated, references deformation, and the like affect only part of a specimen, the
to water shall be understood to mean reagent water as defined presence of process-affected metal in a specimen can affect the
by Type IV of Specification D1193. test result in an unpredictable way depending on the propor-
tions of the area affected.
PRACTICE A—OXALIC ACID ETCH TEST FOR 4.5.3 If the presence of these or other localized conditions is
CLASSIFICATION OF ETCH STRUCTURES OF a concern to the purchaser, then tests that do not average the
AUSTENITIC STAINLESS STEELS (1)7 mass loss over the total specimen surface area, such as Practice
4. Scope A, the Oxalic Acid Etch Test, or Practice E, the Copper–Copper
Sulfate–Sulfuric Acid Test for Detecting Susceptibility to
4.1 The Oxalic Acid Etch Test is used for acceptance of Intergranular Attack in Austenitic Stainless Steels, should be
wrought or cast austenitic stainless steel material but not for considered.
rejection of material. Use of A262 Practice A as a stand-alone
test may reject material that the applicable hot acid test would 5. Summary of Practice
find acceptable; such use is outside the scope of this practice. 5.1 A specimen representative of the material to be evalu-
4.2 This test is intended to be used in connection with other ated is polished to a specified finish and over-etched using
evaluation tests described in these practices to provide a rapid oxalic acid electrolytically. The etched specimen is then
method for identifying qualitatively those specimens that are examined using a metallurgical microscope. The etched struc-
certain to be free of susceptibility to rapid intergranular attack ture is compared with reference photographs to determine
in these other tests. Such specimens have low corrosion rates in whether the material is acceptable or suspect. Suspect material
the various hot acid tests which require from 15 to 240 h of is then subjected to the specified hot acid immersion test.
exposure. These specimens are identified by means of their
etch structures, which are classified according to the criteria 6. Significance and Use
given in Section 11. 6.1 Use of the etch test allows rapid acceptance of specific
4.3 The Oxalic Acid Etch Test may be used to screen lots of material without the need to perform time-consuming
specimens intended for testing in Practice B—Ferric Sulfate- and costly hot acid immersion tests on those lots.
Sulfuric Acid Test, Practice C—Nitric Acid Test, Practice 7. Apparatus
7.1 Etching Cell:
3
Available from American Society of Mechanical Engineers (ASME), ASME 7.1.1 An etching cell may be assembled using components
International Headquarters, Two Park Ave., New York, NY 10016-5990, http://
www.asme.org.
as described in this section. Alternatively, a commercial
4
Available from American Chemical Society (ACS), 1155 Sixteenth St., NW, electropolisher/etcher (as used for metallographic sample
Washington, DC 20036, http://www.acs.org. preparation) may be used for small specimens provided the
5
Available from International Organization for Standardization (ISO), ISO current density requirement of 10.2 is met.
Central Secretariat, Chemin de Blandonnet 8, CP 401, 1214 Vernier, Geneva,
Switzerland, https://www.iso.org. 7.1.2 Source of Direct Current—Battery, generator, or rec-
6
For suggestions on the testing of reagents not listed by the American Chemical tifier capable of supplying about 15 V and 20 A.
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, 7.1.3 Ammeter—For direct current; used to measure the
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
current on the specimen to be etched.
copeial Convention, Inc. (USPC), Rockville, MD.
7
The boldface numbers in parentheses refer to a list of references at the end of 7.1.4 Variable Resistance—Used to control the current on
this standard. the specimen to be etched.

2
 A262 − 15 (2021)
7.1.5 Cathode—A stainless steel container, for example, a 10. Procedure
1 L (1-qt) stainless steel beaker. 10.1 (Warning—Etching should be carried out under a
7.1.5.1 Alternate Cathode—A piece of flat stainless steel at ventilated hood. Gas, which is rapidly evolved at the electrodes
least as large as the specimen surface. with some entrainment of oxalic acid, is poisonous and
7.1.6 Electrical Clamp—To hold the specimen to be etched irritating to mucous membranes.)
and to complete the electrical circuit between the specimen and
the power source such that the specimen is the anode of the 10.2 Etch the polished specimen at 1 A/cm2 for 1.5 min.
cell. 10.2.1 To obtain the correct specified current density:
7.1.7 The power source, resistor, and ammeter must be sized 10.2.1.1 Measure the total immersed area of the specimen to
appropriately for providing and controlling the current as be etched in square centimetres.
specified in 10.2 of this practice. 10.2.1.2 Adjust the variable resistance until the ammeter
reading in amperes is equal to the total immersed area of the
7.1.8 As described, the electrolyte container is the cathode;
specimen in square centimetres.
it may be a stainless steel beaker or fabricated from stainless
steel such as by welding a section of tube or pipe to a flat plate 10.3 A yellow-green film is gradually formed on the cath-
or sheet. Alternatively, the electrolyte container may be glass ode. This increases the resistance of the etching cell. When this
(or other non-conducting, corrosion resisting material) in lieu occurs, remove the film by rinsing the inside of the stainless
of a stainless steel container, and the cathode may be a flat plate steel beaker (or the steel used as the cathode) with an acid such
or sheet of a corrosion resisting alloy. In this latter case, the flat as 30 % HNO3.
surface of the cathode must be at least as large as, facing, and 10.4 The temperature of the etching solution gradually
approximately centered on, the prepared surface of the speci- increases during etching. Keep the temperature below 50 °C.
men. Other configurations of the electrodes might not provide This may be done by alternating two containers. One may be
uniform etching over the specimen surface. In any case, the cooled in tap water while the other is used for etching.
size and shape of the specimen dictate the size and construction
10.4.1 The rate of heating depends on the total current
of the etching cell and of the power source and controls. The
(ammeter reading) passing through the cell. Therefore, keep
overriding principle is that the etch needs to be uniform over
the area to be etched as small as possible while at the same time
the surface to be examined.
meeting the requirements of desirable minimum area to be
7.2 Metallurgical Microscope—For examination of etched etched.
microstructures at 250 to 500 diameters. 10.5 Avoid immersing the clamp holding the specimen in
the etching solution.
8. Reagents and Materials
10.6 Rinsing—Following etching, rinse the specimen thor-
8.1 Etching Solution (10 %)—Dissolve 100 g of reagent oughly in hot water and then in acetone or alcohol to avoid
grade oxalic acid crystals (H2C2O4·2H2O) in 900 mL of crystallization of oxalic acid on the etched surface during
reagent water. Stir until all crystals are dissolved. drying.
8.1.1 Alternate Etching Solution (See 10.7)—Dissolve 100 g
of reagent grade ammonium persulfate ((NH4)2S2O8) in 10.7 It may be difficult to reveal the presence of step
900 mL of reagent water. Stir until dissolved. structures on some specimens containing molybdenum (AISI
316, 316L, 317, 317L), which are free of chromium carbide
sensitization, by electrolytic etching with oxalic acid. In such
9. Sampling and Test Specimens
cases, an alternate electrolyte of ammonium persulfate may be
9.1 The specified hot acid test provides instructions for used in place of oxalic acid. (See 8.1.1.) An etch for 5 or 10
sampling and for specimen preparation such as a sensitization min at 1 A/cm2 in a solution at room temperature readily
heat treatment. Additional instructions specific to Practice A develops step structures on such specimens.
follow:
9.2 The preferred specimen is a cross-section including the 11. Classification of Etch Structures
product surface to be exposed in service. Only such finishing of 11.1 Examine the etched surface on a metallurgical micro-
the product surface should be performed as is required to scope at 250× to 500× for wrought steels and at about 250× for
remove foreign material. cast steels.
9.3 Whenever practical, use a cross-sectional area of 1 cm2 11.2 Examine the etched cross-sectional areas thoroughly
or more. If any cross-sectional dimension is less than 1 cm, by complete traverse from inside to outside diameters of rods
then the other dimension of the cross-section should be a and tubes, from face to face on plates.
minimum of 1 cm. When both dimensions of the product are 11.2.1 Microscopical examination of a specimen shall be
less than 1 cm, use a full cross section. made on metal unaffected by cold-working, carburization,
welding, and the like. If any of these conditions are found, note
9.4 Polishing—On all types of materials, polish cross sec-
their presence in the report.
tional surfaces through CAMI/ANSI 600 [FEPA/ISO P1200] in
accordance with Guide E3 prior to etching and examination. 11.3 Classify the etch structures into the following types
Not all scratches need to be removed. (Note 2):

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 A262 − 15 (2021)

FIG. 1 Step Structure (500×) (Steps Between Grains, No Ditches FIG. 3 Ditch Structure (500×) (One or More Grains Completely
at Grain Boundaries) Surrounded by Ditches)

FIG. 2 Dual Structure (250×) (Some Ditches at Grain Boundaries

FIG. 4 Isolated Ferrite Pools (250×) (Observed in Castings and
in Addition to Steps, but No One Grain Completely Surrounded)
Welds. Steps Between Austenite Matrix and Ferrite Pools)

11.3.1 Step Structure (Fig. 1)—Steps only between grains, 11.3.5 Interdendritic Ditches (Fig. 5)—Observed in castings
no ditches at grain boundaries. and welds. Deep interconnected ditches.
11.3.2 Dual Structure (Fig. 2)—Some ditches at grain 11.3.6 End-Grain Pitting I (Fig. 6)—Structure contains a
boundaries in addition to steps, but no single grain completely few deep end-grain pits along with some shallow etch pits at
surrounded by ditches. 500×. (Of importance only when the nitric acid test is used.)
11.3.3 Ditch Structure (Fig. 3)—One or more grains com- 11.3.7 End-Grain Pitting II (Fig. 7)—Structure contains
pletely surrounded by ditches. numerous, deep end-grain pits at 500×. (Of importance only
11.3.4 Isolated Ferrite (Fig. 4)—Observed in castings and when nitric acid test is used.)
welds. Steps between austenite matrix and ferrite pools. NOTE 2—All photomicrographs were made with specimens that were

4
 A262 − 15 (2021)

FIG. 5 Interdendritic Ditches (250×) (Observed in Castings and NOTE 1—This or a greater concentration of end grain pits at 500× (using
Welds. Deep Interconnected Ditches) standard etching conditions) indicates that the specimen must be tested
when screening is for nitric acid test.
FIG. 7 End Grain Pitting II (500×)

required to determine if there are any grains completely

encircled. If an encircled grain is found, classify the steel as a
ditch structure.
11.4.1 On stainless steel castings (also on weld metal), the
steps between grains formed by electrolytic oxalic acid etching
tend to be less prominent than those on wrought materials or
are entirely absent. However, any susceptibility to intergranular
attack is readily detected by pronounced ditches.
11.4.2 Some wrought specimens, especially from bar stock,
may contain a random pattern of pits. If these pits are sharp and
so deep that they appear black (Fig. 7) it is possible that the
specimen may be susceptible to end grain attack in nitric acid
only. Therefore, even though the grain boundaries all have step
structures, specimens having as much or more end grain pitting
than that shown in Fig. 7 cannot be safely assumed to have low
nitric acid rates and should be subjected to the nitric acid test
whenever it is specified. Such sharp, deep pits should not be
NOTE 1—To differentiate between the types of pits, use a magnification confused with the shallow pits shown in Figs. 1 and 6.
of 500× and focus in the plane of etched surface. The pits which now
appear completely black are end grain pits. 12. Use of Etch Structure Classifications
FIG. 6 End Grain Pitting I (500×) (A Few Deep End Grain Pits
(See 1 in Figure) and Shallow Etch Pits (2)) 12.1 The use of these classifications depends on the hot acid
corrosion test for which stainless steel specimens are being
screened by etching in oxalic acid and is described in each of
the practices.
etched under standard conditions: 10 % oxalic acid, room temperature,
1.5 min at 1 A/cm2. 13. Precision and Bias
11.4 The evaluation of etch structures containing only steps 13.1 Precision and Bias—No information is presented about
and of those showing grains completely surrounded by ditches either the precision or bias of Practice A—Oxalic Acid Etch
in every field can be carried out relatively rapidly. In cases that Test for classification of Etch Structures of Austenitic Stainless
appear to be dual structures, more extensive examination is Steels since the test result is nonquantitative.

5
 A262 − 15 (2021)
PRACTICE B—FERRIC SULFATE–SULFURIC TABLE 1 Use of Etch Structure Classifications from the Oxalic
ACID TEST FOR DETECTING SUSCEPTIBILITY Acid Etch Test with Ferric Sulfate-Sulfuric Acid TestA
Grade Acceptable Etch Suspect
TO INTERGRANULAR ATTACK IN Structures Etch StructuresB
AUSTENITIC STAINLESS STEELS (2)
304 Step, dual, end grain, I & II Ditch
304L Step, dual, end grain, I & II Ditch
14. Scope 316 Step, dual, end grain, I & II Ditch
316L Step, dual, end grain, I & II Ditch
14.1 This practice describes the procedure for conducting 317 Step, dual, end grain, I & II Ditch
the boiling 120-h ferric sulfate–50 % sulfuric acid test which 317L Step, dual, end grain, I & II Ditch
CF-3 Step, dual, isolated ferrite pools Ditch, interdendritic ditches
measures the susceptibility of austenitic stainless steels to CF-8 Step, dual, isolated ferrite pools Ditch, interdendritic ditches
intergranular attack. CF-3M Step, dual, isolated ferrite pools Ditch, interdendritic ditches
CF-8M Step, dual, isolated ferrite pools Ditch, interdendritic ditches
14.2 The presence or absence of intergranular attack in this
A
Grades not listed in this table either have not been evaluated for use of Practice
test is not necessarily a measure of the performance of the A with Practice B or have been found to give acceptable results in the etch test
material in other corrosive environments. The test does not while giving unacceptable results in Practice B. In the latter case Practices A would
provide a basis for predicting resistance to forms of corrosion pass material that should have been subjected to the ferric sulfate-sulfuric acid
test.
other than intergranular, such as general corrosion, pitting, or B
Specimens having these structures shall be tested in the ferric sulfate-sulfuric
stress-corrosion cracking. acid test.

15. Summary of the Ferric Sulfate-Sulfuric Acid Practice

B
intergranular attack in the ferric sulfate-sulfuric acid test. Such
15.1 A specimen representative of the material to be evalu- specimens are acceptable without testing in the ferric sulfate-
ated is immersed in a boiling solution of ferric sulfate and sulfuric acid test. All specimens having suspect etch structures
sulfuric acid for a specified time. The resulting mass loss is shall be tested in the ferric sulfate-sulfuric acid test.
converted to a corrosion rate, which is compared to a specified
maximum value to determine whether the material has the 18. Apparatus
resistance to attack expected of the grade of material being 18.1 The apparatus is illustrated in Fig. 8.
tested.
NOTE 4—Other ground glass joints, such as the 45/40 joint may also be
16. Significance and Use used.

16.1 The ferric sulfate-sulfuric acid test detects susceptibil-

ity to intergranular attack associated primarily with chromium
carbide precipitate in unstabilized austenitic stainless steels,
and to intergranular attack associated with sigma phase.
16.2 The corrosion potential of the ferric sulfate-sulfuric
acid test has been reported as 0.6 V versus a standard calomel
electrode (SCE), as compared with 0.75 to 1.0 V for Practice C,
and 0.1 V for Practices E and F (3).
NOTE 3—A higher corrosion potential indicates more severely oxidizing
conditions.

17. Rapid Screening Test

17.1 Before testing in the ferric sulfate-sulfuric acid test,
specimens of certain grades of stainless steels (see Table 1)
may be given a rapid screening test in accordance with
procedures given in Practice A, Oxalic Acid Etch Test for
Classification of Etch Structures of Austenitic Stainless Steels.
Preparation, etching, and the classification of etch structures
are described therein. The use of etch structure evaluations in
connection with the ferric sulfate-sulfuric acid test is specified
in Table 1.
17.2 Heat treat the material in accordance with 22.1 prior to
performing the etch test.
17.3 Ignore “process-affected” areas (see Section 21); ap-
plication of the ferric sulfate-sulfuric acid test to process-
affected areas is currently outside the scope of Practice B.
17.4 Corrosion test specimens having acceptable etch struc-
tures in the Oxalic Acid Etch Test will be essentially free of FIG. 8 Apparatus for Ferric Sulfate-Sulfuric Acid Test

6
 A262 − 15 (2021)
18.1.1 An Allihn condenser with a minimum of four bulbs 20.1.7 Cover flask with condenser and circulate cooling
and with a ground glass joint to match that of the flask. water.
18.1.1.1 Substitutions for this condenser or flask are not 20.1.8 Boil the solution until all ferric sulfate is dissolved
allowed. Specifically, the cold-finger type of condenser with (see Note 7).
standard Erlenmeyer flasks shall not be used. Corrosion rates 20.1.9 (Warning—It has been reported that violent boiling
obtained using the cold-finger type of condenser are lower than resulting in acid spills can occur. It is important to ensure that
those obtained using the Allihn type of condenser whether due the concentration of acid does not increase and that an adequate
to loss of vapor or to higher oxygen content in the solution or number of boiling chips (which are resistant to attack by the
both. Such lower corrosion rates lead to acceptance of material test solution) are present.)
that should be rejected.
18.1.2 A 1 L Erlenmeyer flask with a ground glass joint to 21. Sampling
match that of the condenser. The flask opening limits the size 21.1 Obtain and prepare only base metal samples.
of the specimen; a larger opening is desirable. 21.1.1 There are two classes of specimens to be considered:
18.1.3 Glass Cradle (Note 5)—Can be supplied by a glass- base metal, and process-affected metal. Process-affected metal
blowing shop. It must be sized so as to fit, with the specimen, contains any condition that affects the corrosion properties of
through the flask opening. It must be designed to allow free the material in a non-uniform way, such as (but not limited to)
flow of the testing solution around the specimen. welds; carburized. nitrided, or oxidized surfaces; mechanical
NOTE 5—Other equivalent means of specimen support, such as glass deformation; and areas affected by heat. Base metal has none
hooks or stirrups, may also be used. of these conditions.
18.1.4 Boiling Chips—Used to prevent bumping. 21.1.2 The Practice B test involves immersing the entire
18.1.5 High Vacuum Silicone Grease—For the ground glass specimen and averaging the mass loss over the entire surface of
joint. the specimen. Welding, carburization, mechanical deformation,
18.1.6 Hot plate, capable of providing heat for continuous and the like, affect only part of a specimen.
boiling of the solution. 21.1.3 The mass loss rate from process-affected metal is
18.1.7 An analytical balance capable of weighing to the expected to differ from that from base metal; the presence of
nearest 0.001 g. process-affected metal in a specimen will affect the calculated
test result in an unpredictable way.
NOTE 6—During testing, there is some deposition of iron oxides on the 21.1.4 If the presence of these or other localized conditions
upper part of the Erlenmeyer flask. This can be readily removed, after test
completion, by boiling a solution of 10 % hydrochloric acid in the flask. is a concern to the purchaser, then tests that do not average the
mass loss over the total specimen surface area, such as Practice
18.1.8 Desiccator—For storage of prepared specimens prior A, the Oxalic Acid Etch Test, or Practice E, the Copper–Copper
to testing. Sulfate–16% Sulfuric Acid Test for Detecting Susceptibility to
Intergranular Attack in Austenitic Stainless Steels, should be
19. Reagents and Materials considered. Details of the test and acceptance criteria shall be
19.1 Ferric Sulfate Hydrate (Fe2(SO4)3·xH2O), about 75 % as agreed by the purchaser and producer.
(Fe2(SO4)3) by mass. 21.2 Unless otherwise specified by the purchaser, the pro-
19.1.1 Ferric sulfate is a specific additive that establishes cedures for obtaining representative base metal samples, for
and controls the corrosion potential. Substitutions are not removing the specimens from the samples, and the number of
permitted. specimens shall be at the discretion of the producer.
19.2 Sulfuric Acid (H2(SO)4), 95.0 to 98.0 % by mass.
22. Preparation of Test Specimens
20. Ferric Sulfate-Sulfuric Acid Test Solution 22.1 Heat treat extra-low carbon and stabilized grades at
20.1 Prepare 600 mL of 50 % (49.4 to 50.9 %) solution as 650 to 675 °C (1200 to 1250 °F), which is the range of
follows: maximum carbide precipitation, prior to testing. The length of
20.1.1 (Warning—Protect the eyes and use rubber gloves time of heating, and the method of subsequent cooling used for
for handling acid. Place the test flask under a hood.) this sensitizing treatment together with the corresponding
20.1.2 First, measure 400.0 mL of Type IV reagent water maximum permissible corrosion rate shall be as agreed be-
and pour into the Erlenmeyer flask. tween the material producer and purchaser.
20.1.3 Then measure 236.0 mL of reagent-grade sulfuric NOTE 8—The most commonly used sensitizing treatment is 1 h at
acid. Add the acid slowly and with constant stirring to the 675 °C (1250 °F).
water in the Erlenmeyer flask to avoid boiling by the heat 22.2 Prepare the specimens, each having a total surface area
evolved. of 5 to 20 cm2.
NOTE 7—Loss of vapor results in concentration of the acid. 22.3 Where feasible for the product form, grind all the
20.1.4 Weigh 25 g of reagent-grade ferric sulfate to the specimen surfaces using CAMI/ANSI 120 [FEPA/ISO P120]
nearest 0.1 g and add to the sulfuric acid solution. paper-backed, wet or dry, closed coated abrasive paper, with
20.1.5 Drop boiling chips into the flask. water as a coolant. If abrasive paper is used dry, polish slowly
20.1.6 Lubricate ground glass joint with silicone grease. to avoid overheating. Do not use abrasives with grinding aids;

7
 A262 − 15 (2021)
some grinding aids contain fluorides that can affect the 23.13 Several specimens may be tested simultaneously. The
measured corrosion rate. number (3 or 4) is limited only by the number of glass cradles
that can be fitted into the flask.
22.4 Remove all traces of oxide scale and heat tint formed
during heat treatments. Any scale that cannot be removed by 24. Calculation and Report
grinding (for example, in stamped numbers) may be removed
by using one of the pickling solutions described in Practice 24.1 The effect of the acid solution on the material is
A380/A380M, Table A1.1. (Residual oxide scale causes gal- measured by determining the loss of weight of the specimen.
vanic action and consequent activation in the test solution.) The corrosion rates should be reported as millimetres of
penetration per month (Note 9), calculated as follows:
22.5 Measure the specimens, including the inner surfaces of Millimetre per month 5 ~ 7305 3 W ! / ~ A 3 t 3 d ! (1)
any holes, to the nearest 0.05 mm (0.001 in.) and calculate the
total exposed area. where:
22.6 Degrease the specimens using suitable nonchlorinated t = time of exposure, h,
A = area, cm2,
agents, such as soap and lukewarm water, or acetone. Dry the
W = weight loss, g, and
specimens and weigh each one to the nearest 0.001 g. Store the d = density, g/cm3
specimens in a desiccator until the test is to be performed.
for chromium-nickel steels, d = 7.9 g/cm3
23. Procedure for chromium-nickel-molybdenum steels, d = 8.00 g/cm3
NOTE 9—Conversion factors to other commonly used units for corro-
23.1 If the test solution is not already boiling, bring it to sion rates are as follows:
boiling. Millimetres per month × 0.04 = inches per month
23.1.1 Keep the flask covered with the condenser (with Millimetres per month × 0.47 = inches per year
cooling water flowing) except when inserting or removing Millimetres per month × 12 = millimetres per year
Millimetres per month × 472 = mils per year
specimens. (See Note 7.) Millimetres per month × 1000 × density/3 = milligrams per square
23.2 Turn off the heat source and allow the boiling to decimetre per day
Millimetres per month × 1.39 × density = grams per square metre per hour
subside.
23.3 Place specimens in glass cradles. 25. Precision and Bias
25.1 Precision—The precision of Practice B is being deter-
23.4 Uncover the flask.
mined.
23.5 Insert the specimens. 25.2 Bias—This practice has no bias because the resistance
23.6 Replace the condenser immediately, restore cooling to intergranular corrosion is defined only in terms of this
water flow, and turn on the heat source. practice.
23.7 Mark the liquid level on the flask to provide a check on PRACTICE C—NITRIC ACID TEST FOR
vapor loss, which would result in concentration of the acid. If DETECTING SUSCEPTIBILITY TO
there is an appreciable change in the level, repeat the test with INTERGRANULAR ATTACK IN
fresh solution and reground and reweighed specimens. AUSTENITIC STAINLESS STEELS
23.8 Continue the immersion of the specimens for a total of 26. Scope
120 h (five days), then remove the specimens, rinse in water or
acetone, and dry. 26.1 This practice describes the procedure for conducting
the boiling nitric acid test (2) as employed to measure the
23.9 Weigh the specimens and subtract the new weights relative susceptibility of austenitic stainless steels to inter-
from original weights. granular attack.
23.10 Intermediate weighings are usually not necessary. The 26.2 The presence or absence of intergranular attack in this
test can be run without interruption for 120 h. However, if test is not necessarily a measure of the performance of the
preliminary results are desired, the specimens can be removed material in other corrosive environments; in particular, it does
at any time for weighing. not provide a basis for predicting resistance to forms of
corrosion other than intergranular, such as general corrosion,
23.11 Changes to the solution during the 120-h test periods pitting, or stress-corrosion cracking.
are not necessary.
23.12 If the corrosion rate is extraordinarily high, as evi- 27. Summary of Test Method C, the Nitric Acid Test
denced by a change in the color (from yellow to green) of the 27.1 A specimen representative of the material to be evalu-
solution, additional ferric sulfate inhibitor may need to be ated is immersed in a boiling solution of nitric acid for a
added during the test. If the total weight loss of all the specified time. The resulting mass loss is converted to a
specimens in a flask exceeds 2 g, more ferric sulfate must be corrosion rate, which is compared to a specified maximum
added. (During the test, ferric sulfate is consumed at a rate of value to determine whether the material has the resistance to
10 g for each 1 g of dissolved stainless steel.) attack expected of the grade of material being tested.

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 A262 − 15 (2021)
28. Significance and Use
28.1 The nitric acid test detects susceptibility to rapid
intergranular attack associated with chromium carbide precipi-
tate
28.2 The corrosion potential of the nitric acid test (Practice
C) has been reported as 0.75 to 1.0 V versus a standard calomel
electrode as compared with 0.6 V for Practice B, and 0.1 V for
Practices E and F. (3).
NOTE 10—Higher corrosion potential indicates more severely oxidizing
conditions. The high corrosion potential of the nitric acid test suggests that
it should be invoked only when the material is destined for nitric acid
service.

29. Rapid Screening Test

29.1 Before testing in the nitric acid test, specimens of
certain grades of stainless steel, as given in Table 2, may be FIG. 9 Flask and Condenser for Nitric Acid Test
given a rapid screening test in accordance with procedures
given in Practice A, Oxalic Acid Etch Test for Classification of
Etch Structures of Austenitic Stainless Steels. The use of the 30.4 Balance—An analytical balance capable of weighing
etch structure evaluations in connection with the nitric acid test to at least the nearest 0.001 g.
is specified in Table 2. 30.5 Desiccator—For storage of prepared specimens prior
29.2 Heat treat the material in accordance with 33.1 prior to to testing.
performing the etch test.
31. Nitric Acid Test Solution
29.3 Ignore “process-affected” areas, if any (see Section
31.1 The test solution shall be 65.0 6 0.2 weight % as nitric
32); application of the nitric acid test to process-affected areas
acid determined by analysis.
is currently outside the scope of Practice C.
31.2 Prepare this solution by adding reagent grade nitric
29.4 Corrosion test specimens having acceptable etch struc-
acid (HNO3 Table 3) to reagent water at the rate of 108 mL of
tures in the Oxalic Acid Etch Test will be essentially free of
reagent water per litre of reagent nitric acid.
intergranular attack in the nitric acid test; such specimens are
acceptable without testing in the nitric acid test. All specimens 31.3 (Warning—Protect the eyes and use rubber gloves for
having suspect etch structures shall be tested in the nitric acid handling acid. Place the test flask under a hood.)
test. 31.4 The nitric acid used shall conform to the American
Chemical Society Specifications for Reagent Chemicals and
30. Apparatus the additional requirements of this test method as shown in
30.1 Container—A 1 L Erlenmeyer flask equipped with a Table 3.
cold finger-type condenser, as illustrated in Fig. 9.
32. Sampling
30.2 Specimen Supports—Glass hooks, stirrups, or cradles
for supporting the specimens in the flask fully immersed at all 32.1 Obtain and prepare only base metal samples.
times during the test and so designed that specimens tested in 32.1.1 There are two classes of specimens to be considered:
the same container do not come in contact with each other. base metal, and process-affected metal. Process-affected metal
contains any condition that affects the corrosion properties of
30.3 Heater—A means for heating the test solutions and of
the material in a non-uniform way, such as (but not limited to)
keeping them boiling throughout the test period. An electrically
welds; carburized. nitrided, or oxidized surfaces; mechanical
heated hot plate is satisfactory for this purpose.
deformation; and areas affected by heat. Base metal has none
of these conditions.
TABLE 2 Use of Etch Structure Classification from Oxalic Acid
Etch Test with Nitric Acid TestA
Acceptable Etch Suspect Etch TABLE 3 Nitric Acid Composition Limits
Grade
Structures StructuresB
Minimum Maximum
AISI 304 Step, dual, end grain I Ditch, end grain II
Nitric Acid (HNO3), mass percent 69.0 71.0
AISI 304L Step, dual, end grain I Ditch, end grain II
Ash, ppm { 5
ACI CF-8 Step, dual, isolated ferrite pools Ditch, interdendritic ditches
Chloride as Cl, ppm { 0.5
ACI CF-3 Step, dual, isolated ferrite pools Ditch, interdendritic ditches
Sulfate, as (SO4), ppm { 1
A Arsenic (As), ppm 0.01
Grades not listed in this table either have not been evaluated for use of Practice {
A with Practice B or have been found to give acceptable results in the etch test Heavy metals, as Pb, ppm { 0.2
while giving unacceptable results in Practice B. In the latter case Practice A would Iron, (Fe), ppm { 0.2
pass material that should have been subjected to the ferric sulfate-sulfuric acid Additional limits per Practices A262
test. Fluorine (F), ppm { 1
B
Specimens having these structures shall be tested in the nitric acid test. Phosphate (PO4), ppm { 0.2

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 A262 − 15 (2021)
32.1.2 The Practice C test involves immersing the entire 33.5 Degrease the specimen using suitable nonchlorinated
specimen and averaging the mass loss over the entire surface of agents, such as soap and lukewarm water, or acetone (Note 13).
the specimen. Welding, carburization, mechanical deformation, Dry the specimens and weigh each one to the nearest 0.001 g.
and the like, affect only part of a specimen. Store the specimens in a desiccator until the test is to be
32.1.3 The mass loss rate from process-affected metal is performed.
expected to differ from that from base metal; the presence of NOTE 13—The cleaning treatment described may be supplemented by
process-affected metal in a specimen will affect the calculated immersing the specimen in nitric acid (for example, 20 weight % at 49 to
test result in an unpredictable way. 60 °C (120 to 140 °F)) for 20 min, followed by rinsing, drying, and
32.1.4 If the presence of these or other localized conditions weighing. In the case of small-diameter tubular specimens which cannot
is a concern to the purchaser, then tests that do not average the be conveniently resurfaced on the inside, it is desirable to include in the
preparation an immersion in boiling nitric acid (65 %) for 2 to 4 h using
mass loss over the total specimen surface area, such as Practice the same apparatus as for the actual test. The purpose of these treatments
A, the Oxalic Acid Etch Test, or Practice E, the Copper–Copper is to remove any surface contamination that may not be accomplished by
Sulfate–Sulfuric Acid Test for Detecting Susceptibility to the regular cleaning method and which may increase the apparent weight
Intergranular Attack in Austenitic Stainless Steels, should be loss of the specimen during the early part of the test.
considered. Details of the test and acceptance criteria shall be 33.6 The standard test is to test only one specimen of each
as agreed by the purchaser and producer. material or lot of material. However, in case of dispute, the use
32.2 Unless otherwise specified by the purchaser, the pro- of at least two specimens for check purposes is recommended.
cedures for obtaining representative base metal samples, for
removing the specimens from the samples, and the number of 34. Procedure
specimens shall be at the discretion of the producer. 34.1 Use a sufficient quantity of the nitric acid test solution
32.3 When specimens are cut by shearing, the sheared edges to cover the specimens and to provide a volume of at least 20
shall be refinished by machining or grinding prior to testing. mL/cm2 (125 mL/in.2) of specimen surface. Normally, a
volume of about 600 mL is used.
33. Preparation of Test Specimens 34.2 Use a separate container for each test specimen.
33.1 Heat treat extra-low carbon and stabilized grades at 34.2.1 As many as three specimens may be tested in the
650 to 675 °C (1200 to 1250 °F), which is the range of same container provided that they all are of the same grade and
maximum carbide precipitation, prior to testing. The length of all show satisfactory resistance to corrosion.
time of heating, and the method of subsequent cooling used for 34.2.2 If more than one of the specimens tested in the same
this sensitizing treatment together with the corresponding container fail to pass the test, retest all the specimens in
maximum permissible corrosion rate shall be as agreed be- separate containers.
tween the material producer and purchaser. NOTE 14—Excessive corrosion of one specimen may result in acceler-
ated corrosion of the other specimens tested with it. Excessive corrosion
NOTE 11—The most commonly used sensitizing treatment is 1 h at may often be detected by changes in the color of the test solution, and it
675 °C (1250 °F). may be appropriate to provide separate containers for such specimens
NOTE 12—The size and shape of the specimen must be considered with without waiting until the end of the test period. A record should be made
respect to available facilities for accurate weighing and the volume of test showing which specimens were tested together.
solution to be used. Normally, the maximum convenient weight of a
specimen is about 100 g. In the case of bar, wire, and tubular products, the 34.3 After the specimens have been placed in the acid in the
proportion of the total area represented by the exposed cross section may container, pass cooling water through the condenser, bring the
influence the results. Cross-sectional areas in these products may be acid to a boil on the hot plate, and keep boiling throughout the
subject to end grain attack in nitric acid. The proportion of end grain in the test period (Note 15). After each test period, rinse the speci-
specimen should therefore be kept low unless such surface is actually to
be exposed in service involving nitric acid. In this latter case, the mens with water and treat by scrubbing with rubber or a nylon
proportion of end grain in the specimen should be kept high. brush under running water to remove any adhering corrosion
33.2 Where feasible for the product form, grind all the products, then dry and weigh them. Drying may be facilitated,
specimen surfaces using CAMI/ANSI 120 [FEPA/ISO P120] if desired, by dipping the specimens in acetone after they are
paper-backed, wet or dry, closed coated abrasive paper, with scrubbed.
water as a coolant. If abrasive paper is used dry, polish slowly 34.4 (Warning—It has been reported that violent boiling
to avoid overheating. Do not use abrasives with grinding aids; resulting in acid spills can occur. It is important to ensure that
some grinding aids contain fluorides that can affect the the concentration of acid does not increase and that an adequate
measured corrosion rate. number of boiling chips (which are resistant to attack by the
test solution) are present.)
33.3 Remove all traces of oxide scale and heat tint formed
during heat treatments. Any scale that cannot be removed by NOTE 15—Take care to prevent contamination of the testing solution,
grinding (for example, in stamped numbers) may be removed especially by fluorides, either before or during the test. Experience has
by using one of the pickling solutions described in Practice shown that the presence of even small amounts of hydrofluoric acid will
increase the corrosion rate in the nitric acid test. It is not permissible, for
A380/A380M, Table A1.1. example, to conduct nitric-hydrofluoric acid tests in the same hood with
33.4 Measure the specimen, including the inner surfaces of nitric acid tests.
any holes to the nearest 0.05 mm (0.001 in.), and calculate the 34.5 The standard test consists of five boiling periods of
total exposed area in cm2. 48 h each with a fresh test solution being used in each period.

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 A262 − 15 (2021)
34.5.1 A combination of one 48-h period and two 96-h TABLE 4 Use of Etch Structure Classifications from the Oxalic
periods (not necessarily in that order) instead of five 48-h test Acid Etch Test with the Copper–Copper Sulfate–16 % Sulfuric
Acid Test
periods may be used if so agreed by the purchaser.
Acceptable Etch Suspect Etch
Grade
Structures Structures A
35. Calculation and Report
AISI 201 Step, dual, end grain I and II Ditch
35.1 Calculation—The effect of the acid on the material AISI 202 Step, dual, end grain I and II Ditch
shall be measured by determining the loss of weight of the AISI 301 Step, dual, end grain I and II Ditch
AISI 304 Step, dual, end grain I and II Ditch
specimen after each test period and for the total of the test AISI 304L Step, dual, end grain I and II Ditch
periods. Using Eq 1, calculate the corrosion rate for each AISI 304H Step, dual, end grain I and II Ditch
specimen for each test period, and for the total of the test AISI 316 Step, dual, end grain I and II Ditch
AISI 316L Step, dual, end grain I and II Ditch
periods. AISI 316H Step, dual, end grain I and II Ditch
AISI 317 Step, dual, end grain I and II Ditch
35.2 Report—Report the calculated corrosion rates for the AISI 317L Step, dual, end grain I and II Ditch
individual periods in chronological order, as well as the AISI 321 Step, dual, end grain I and II Ditch
average for the five test periods. If the modified test periods AISI 347 Step, dual, end grain I and II Ditch
(34.5.1) are used, then identify each result as to the sequence A
Specimens having these structures must be tested in the copper–copper
and length of the test period. sulfate–16 % sulfuric acid test.

36. Precision and Bias

36.1 Precision—The precision of Practice C is being deter- 39. Summary of Practice
mined.
39.1 A suitable sample of an austenitic stainless steel,
36.2 Bias—This practice has no bias because the resistance embedded in copper shot or grindings, is exposed to boiling
to intergranular corrosion is defined only in terms of this acidified copper sulfate solution for 15 h. After exposure in the
practice. boiling solution, the specimen is bent. Intergranular cracking or
PRACTICE E—COPPER-COPPER SULFATE–16 % crazing is evidence of susceptibility.
SULFURIC ACID TEST FOR DETECTING 39.2 Alternative Testing Procedures:
SUSCEPTIBILITY TO INTERGRANULAR 39.2.1 Unless prohibited by the purchaser in the purchase
ATTACK IN AUSTENITIC STAINLESS STEELS (4, 5) order, the supplier is permitted to meet the requirements of
Practice E by performing a test in accordance with ISO 3651-2,
37. Scope Method A, provided that the testing period shall be a minimum
37.1 This practice describes the procedure by which the of 15 h. When a sensitization treatment is required, sensitiza-
copper–copper sulfate–16 % sulfuric acid test is conducted to tion heat treatment T1 [700 6 10 °C (1292 6 18 °F), 30 min,
determine the susceptibility of austenitic stainless steels to water quench] shall be used unless the supplier and purchaser
intergranular attack. The presence or absence of intergranular shall agree upon preparation of welded test pieces to be tested
corrosion in this test is not necessarily a measure of the in the as-welded condition.
performance of the material in other corrosive media. The test 39.2.2 When this alternative test procedure is used, it shall
does not provide a basis for predicting resistance to other forms be noted on the test report.
of corrosion, such as general corrosion, pitting, or stress-
corrosion cracking. 40. Apparatus
40.1 The basic apparatus is described in Section 18.
38. Rapid Screening Test
40.2 Specimen Supports—An open glass cradle capable of
38.1 Before testing in the copper–copper sulfate–16 % sul- supporting the specimens and copper shot or grindings in the
furic acid test, specimens of certain grades of stainless steel flask is recommended.
(see Table 4) may be given a rapid screening test in accordance
with the procedures given in Practice A (Sections 4 through NOTE 16—It may be necessary to embed large specimens, such as from
heavy bar stock, in copper shot on the bottom of the test flask. A copper
13). Preparation, etching, and the classification of etch struc- cradle may also be used.
tures are described therein. The use of etch-structure evalua-
tions in connection with the copper–copper sulfate–16 % 40.3 Heat Source—Any gas or electrically heated hot plate
sulfuric acid test is specified in Table 4. may be utilized for heating the test solution and keeping it
38.1.1 Corrosion test specimens having acceptable etch boiling throughout the test period.
structures in the Oxalic Acid Etch Test will be essentially free 41. Acidified Copper Sulfate Test Solution
of intergranular attack in the copper–copper sulfate–16 %
sulfuric acid test. Such specimens are acceptable without 41.1 Dissolve 100 g of reagent grade copper sulfate
testing in the copper–copper sulfate–16 % sulfuric acid test. All (CuSO4·5H2O) in 700 mL of distilled water, add 100 mL of
specimens having suspect etch structures must be tested in the sulfuric acid (H2SO4, cp, sp gr 1.84), and dilute to 1000 mL
copper–copper sulfate–16 % sulfuric acid test. with distilled water.
38.1.2 Heat treat the material when required by and in NOTE 17—The solution will contain approximately 6 weight % of
accordance with 43.3.1 prior to performing the etch test. anhydrous CuSO4 and 16 weight % of H2SO4.

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 A262 − 15 (2021)
42. Copper Addition 43.2 Any scale on the specimens should be removed me-
42.1 Electrolytic grade copper shot or grindings may be chanically unless a particular surface finish is to be evaluated.
used. Shot is preferred for its ease of handling before and after Chemical removal of scale is permissible when this is the case.
the test. Mechanical removal of scale should be accomplished with
120-grit iron-free aluminum oxide abrasive.
42.2 A sufficient quantity of copper shot or grindings is to 43.2.1 Each specimen should be degreased using a cleaning
be used to cover all surfaces of the specimen whether it is in a solvent such as acetone, alcohol, ether, or a vapor degreaser
vented glass cradle or embedded in a layer of copper shot on prior to being tested.
the bottom of the test flask.
43.3 All austenitic material in the “as-received” (mill-
42.3 The amount of copper used, assuming an excess of annealed) condition should be capable of meeting this test.
metallic copper is present, is not critical. The effective galvanic 43.3.1 Specimens of extra-low-carbon and stabilized grades
coupling between copper and the test specimen may have are tested after sensitizing heat treatments at 650 to 675 °C
importance (6). (1200 to 1250 °F), which is the range of maximum carbide
42.4 The copper shot or grindings may be reused if they are precipitation. The most commonly used sensitizing treatment is
cleaned in warm tap water after each test. 1 h at 675 °C. Care should be taken to avoid carburizing or
nitriding the specimens. The heat treating is best carried out in
43. Specimen Preparation air or neutral salt.
43.1 The size of the sample submitted for test and the area NOTE 18—The sensitizing treatment 675 °C is performed to check the
from which it is to be taken (end or middle of coil, midway effectiveness of stabilized and 0.03 % maximum carbon materials in
surface and center, and so forth) is generally specified in the resisting carbide precipitation, hence, intergranular attack.
agreement between the purchaser and the seller. The testing
44. Test Conditions
apparatus dictates the final size and shape of the test specimen.
The specimen configuration should permit easy entrance and 44.1 The volume of acidified copper sulfate test solution
removal through the neck of the test container. used should be sufficient to completely immerse the specimens
43.1.1 Table 5 may be used as a guide to determine and provide a minimum of 8 mL/cm2 (50 mL/in.2) of specimen
acceptable specimen sizes. There may be restrictions placed on surface area.
specimen size by the testing apparatus. 44.1.1 As many as three specimens can be tested in the same
43.1.2 Specimens obtained by shearing should have the container. It is ideal to have all the specimens in one flask to be
sheared edges machined or ground off prior to testing. Care of the same grade, but it is not absolutely necessary. The
should be taken when grinding to avoid overheating or solution volume-to-sample area ratio is to be maintained.
“burning.” A “squared” edge is desirable. 44.1.2 The test specimen(s) should be immersed in ambient
test solution, which is then brought to a boil and maintained
boiling throughout the test period. Begin timing the test period
TABLE 5 Sizes of Test Specimens when the solution reaches the boiling point.
Type of Material Size of Test Specimen
NOTE 19—Measures should be taken to minimize bumping of the
Wrought wire or rod:
Up to 6 mm (¼ in.) in diameter, incl Full diameter by 75 mm (3 in.) (min) solution when glass cradles are used to support specimens. A small
long amount of copper shot (eight to ten pieces) on the bottom of the flask will
Over 6 mm (¼ in.) in diameter Cylindrical segment 6 mm (¼ in.) thick conveniently serve this purpose.
by 25 mm (1 in.) (max) wide by 75
to 125 mm (3 to 5 in.) longA
44.1.3 The time of the test shall be a minimum of 15 h,
unless a longer time is agreed upon between the purchaser and
Wrought sheet, strip, plates, or flat the producer. If not 15 h, the test time shall be specified on the
rolled products:
Up to 5 mm (3⁄16 in.) thick, incl Full thickness by 9 to 25 mm (" to
test report. Fresh test solution would not be needed if the test
1 in.) wide by 75 mm (3 in.) (min) were to run 48 or even 72 h. (If any adherent copper remains
long on the specimen, it may be removed by a brief immersion in
Over 5 mm (3⁄16 in.) thick 5 to 13 mm (3⁄16 to ½ in.) thick by
9 to 25 mm (" to 1 in.) wide by concentrated nitric acid at room temperature.)
75 mm (3 in.) (min) longB
NOTE 20—Results in the literature indicate that this test is more
Tubing: sensitive if it is run for longer times (3, 7).
Up to 38 mm (1½ in.) in diameter, incl Full ring, 25 mm (1 in.) wide C
Over 38 mm (1½ in.) in diameter A circumferential segment 75 mm 45. Bend Test
(3 in.) (min) long cut from a 25 mm
(1-in.) wide ringD 45.1 The test specimen shall be bent through 180° and over
A
When bending such specimens, the curved surface shall be on the outside of the
a diameter equal to the thickness of the specimen being bent
bend. (see Fig. 10). In no case shall the specimen be bent over a
B
One surface shall be an original surface of the material under test and it shall be smaller radius or through a greater angle than that specified in
on the outside of the bend. Cold-rolled strip or sheets may be tested in the
thickness supplied.
the product specification. In cases of material having low
C
Ring sections are not flattened or subjected to any mechanical work before they ductility, such as severely cold worked material, a 180° bend
are subjected to the test solution. may prove impractical. Users shall inform those conducting the
D
Specimens from welded tubes over 38 mm (1½ in.) in diameter shall be taken
with the weld on the axis of the bend. Practice E test when the material is in the low ductility highly
stressed condition, such as highly cold worked material.

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 A262 − 15 (2021)
45.1.5.4 Face, root, or side bend tests may be performed,
and the type of bend test shall be agreed upon between the
purchaser and the producer. The bend radius shall not be less
than that required for mechanical testing in the appropriate
material specification (for base metal) or in ASME Code
Section IX (for welds).
46. Evaluation
46.1 The bent specimen shall be examined under low (5 to
20×) magnification (see Fig. 11). The appearance of fissures or
cracks indicates the presence of intergranular attack (see Fig.
12).
46.1.1 When an evaluation is questionable (see Fig. 13), the
presence or absence of intergranular attack shall be determined
by the metallographic examination of the outer radius of a
longitudinal section of the bend specimen at a magnification of
100 to 250×.
FIG. 10 A Bent Copper–Copper Sulfate–Sulfuric Acid 46.1.2 Cracking that originates at the edge of the specimen
Test Specimen shall be disregarded. The appearance of deformation lines,
wrinkles, or “orange peel” on the surface, without accompa-
Determine the maximum angle of bend without causing cracks
nying cracks or fissures, shall be disregarded also.
in such material by bending an untested specimen of the same
46.1.3 Cracks suspected as arising through poor ductility
configuration as the specimen to be tested. After exposure to
shall be investigated by bending a similar specimen that was
the acidified copper–copper sulfate sulfuric acid test solution,
not exposed to the boiling test solution. A visual comparison
the maximum angle of bend without causing cracks as deter-
between these specimens should assist in interpretation.
mined from untested low ductility specimens shall be utilized
in evaluation of the specimens exposed to the acidified PRACTICE F—COPPER-COPPER SULFATE–50 %
copper–copper sulfate sulfuric acid test solution. The angle of SULFURIC ACID TEST FOR DETERMINING
bend utilized in evaluating tested specimens shall be reported. SUSCEPTIBILITY TO INTERGRANULAR ATTACK
45.1.1 Duplicate specimens shall be obtained from sheet IN AUSTENITIC STAINLESS STEELS
material so that both sides of the rolled samples may be bent.
This will assure detection of intergranular attack resulting from 47. Scope
carburization of one surface of sheet material during the final 47.1 This practice describes the procedure for conducting
stages of rolling. the boiling copper–copper sulfate–50 % sulfuric acid test,
NOTE 21—Identify the duplicate specimen in such a manner as to which measures the susceptibility of stainless steels to inter-
ensure both surfaces of the sheet material being tested are subjected to the granular attack.
tension side of the bends.
47.2 The presence or absence of intergranular attack in this
45.1.2 Samples machined from round sections or cast ma- test is not necessarily a measure of the performance of the
terial shall have the curved or original surface on the outside of material in other corrosive environments. The test does not
the bend. provide a basis for predicting resistance to forms of corrosion
45.1.3 The specimens are generally bent by holding in a vise other than intergranular, such as general corrosion, pitting, or
and starting the bend with a hammer. It is generally completed stress-corrosion cracking.
by bringing the two ends together in the vise. Heavy specimens
may require bending in a fixture of suitable design. An air or 48. Summary of Test Method F, Copper–Copper
hydraulic press may also be used for bending the specimens. Sulfate–50% Sulfuric Acid Test
45.1.4 Tubular products should be flattened in accordance 48.1 A specimen representative of the material to be evalu-
with the flattening test, prescribed in Test Methods and ated is immersed in a boiling solution of copper sulfate and
Definitions A370. sulfuric acid for a specified time. A piece of copper is also
45.1.5 When agreed upon between the purchaser and the immersed in the solution to maintain a constant corrosion
producer, the following shall apply to austenitic stainless steel potential. The resulting mass loss is converted to a corrosion
plates 4.76 mm (0.1875 in.) and thicker: rate, which is compared to a specified maximum value to
45.1.5.1 Samples shall be prepared according to Table 5. determine whether the material has the resistance to attack
45.1.5.2 The radius of bend shall be two times the sample expected of the grade of material being tested.
thickness, and the bend axis shall be perpendicular to the
direction of rolling. 49. Significance and Use
45.1.5.3 Welds on material 4.76 mm (0.1875 in.) and thicker 49.1 The copper–copper sulfate–sulfuric acid test detects
shall have the above bend radius, and the weld-base metal susceptibility to intergranular attack associated primarily with
interface shall be located approximately in the centerline of the chromium carbide precipitate in unstabilized cast austenitic
bend. stainless steels and in certain wrought grades.

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 A262 − 15 (2021)

FIG. 11 Passing Test Specimen—View of the Bent Area (20× Magnification Before Reproduction)

FIG. 12 Failing Test Specimen (Note the many intergranular fissures. Bent Area at 20× Magnification Before Reproduction.)

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 A262 − 15 (2021)

FIG. 13 Note the Traces of Intergranular Fissures and “Orange-Peel” Surface. Bent Area at 20× Magnification
Before Reproduction.)

49.2 The copper–copper sulfate–sulfuric acid test does not are described therein. The use of etch structure evaluations in
detect susceptibility to intergranular attack associated primarily connection with the copper–copper sulfate–50 % sulfuric acid
with sigma phase. test is specified in Table 6.
49.3 The corrosion potential of the copper–copper sulfate- 50.2 Heat treat the material in accordance with 55.1 prior to
–sulfuric acid test has been reported as 0.1 V as compared with performing the etch test.
0.6 V for Practice B, 0.75 to 1.0 V for Practice C, and 0.1 V for 50.3 Ignore “process-affected” areas (see 54.1.1); applica-
Practice E. (3) tion of the etch test to these areas is currently outside the scope
NOTE 22—Higher corrosion potential indicates more severely oxidizing of Practice F.
conditions.
50.4 Corrosion test specimens having acceptable etch struc-
50. Rapid Screening Test tures in the Oxalic Acid Etch Test will be essentially free of
intergranular attack in the copper–copper sulfate–50 % sulfuric
50.1 Before testing in the copper–copper sulfate–50 % sul- acid test. Such specimens are acceptable without testing in the
furic acid test, specimens of certain grades of stainless steels copper–copper sulfate–50 % sulfuric acid test. All specimens
(see Table 6) may be given a rapid screening test in accordance having suspect etch structures shall be tested in the copper-
with procedures given in Practice A, Oxalic Acid Etch Test for –copper sulfate–50 % sulfuric acid test.
Classification of Etch Structures of Austenitic Stainless Steels.
Preparation, etching, and the classification of etch structures 51. Apparatus
51.1 The basic apparatus is described in Section 18.
TABLE 6 Use of Etch Structure Classifications from the Oxalic
51.1.1 Substitutions for this condenser or flask are not
Acid Etch Test With the Copper–Copper Sulfate–50 % Sulfuric
Acid TestA allowed. Specifically, the cold-finger type of condenser with
Grade Acceptable Etch Structures Suspect Etch StructuresB standard Erlenmeyer flasks shall not be used. Corrosion rates
CF-3M Step, dual, isolated ferrite Ditch, interdendritic ditches obtained using the cold-finger type of condenser are lower than
CF-8M Step, dual, isolated ferrite Ditch, interdendritic ditches those obtained using the Allihn type of condenser whether due
A
Grades not listed in this table either have not been evaluated for use of Practice to loss of vapor or to higher oxygen content in the solution or
A with Practice F or have been found to give acceptable results in the etch test both.
while giving unacceptable results in Practice F. In the latter case Practice A would
pass material that should have been subjected to the copper–copper sulfate-
sulfuric acid test. 52. Reagents and Materials
B
Specimens having these structures shall be tested in the copper–copper
sulfate-sulfuric acid test 52.1 Cupric Sulfate Pentahydrate (CuSO4·5H2O); about
64 % (CuSO4) by mass.

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 A262 − 15 (2021)
52.1.1 Cupric sulfate is a specific additive that establishes A, the Oxalic Acid Etch Test, or Practice E, the Copper–Copper
and controls the corrosion potential. Substitutions are not Sulfate–16% Sulfuric Acid Test for Detecting Susceptibility to
permitted. Intergranular Attack in Austenitic Stainless Steels, should be
52.2 Sulfuric Acid (H2SO4), 95.0 to 98.0 % by mass. considered. Details of the test and acceptance criteria shall be
as agreed by the purchaser and producer.
52.3 A piece of copper metal about 3 by 20 by 40 mm (1⁄8
by 3⁄4 by 11⁄2 in.) with a bright, clean finish. An equivalent area 54.2 Unless otherwise specified by the purchaser, the pro-
of copper shot or chips may be used. cedures for obtaining representative base metal samples, for
52.3.1 Wash, degrease, and dry the copper before use. removing the specimens from the samples, and the number of
specimens shall be at the discretion of the producer.
NOTE 23—A rinse in 5 % H2SO4 will clean corrosion products from the
copper.
55. Preparation of Test Specimens
53. Copper–Copper Sulfate–50 % Sulfuric Acid Test 55.1 Heat treat extra-low carbon and stabilized grades at
Solution 650 to 675 °C (1200 to 1250 °F), which is the range of
53.1 Prepare 600 mL of test solution as follows: maximum carbide precipitation, prior to testing. The length of
53.1.1 (Warning—Protect the eyes and face by face shield time of heating, and the method of subsequent cooling used for
and use rubber gloves and apron when handling acid. Place this sensitizing treatment together with the corresponding
flask under hood.) maximum permissible corrosion rate shall be as agreed be-
53.1.2 First, measure 400.0 mL of Type IV reagent water tween the material producer and purchaser.
and pour into the Erlenmeyer flask. NOTE 24—The most commonly used sensitizing treatment is 1 h at
53.1.3 Then measure 236.0 mL of reagent grade sulfuric 675 °C (1250 °F).
acid. Add the acid slowly to the water in the Erlenmeyer flask
55.2 Prepare the specimens, each having a total surface area
to avoid boiling by the heat evolved. (Note 7.)
of 5 to 20 cm2.
53.1.4 Weigh 72 g of reagent grade copper sulfate (CuSO4·5
H2O) and add to the sulfuric acid solution. 55.3 Where feasible for the product form, grind all the
53.1.5 Place the copper piece into one glass cradle and put specimen surfaces using CAMI/ANSI 120 [FEPA/ISO P120]
it into the flask. paper-backed, wet or dry, closed coated abrasive paper, with
53.1.6 Drop boiling chips into the flask. water as a coolant. If abrasive paper is used dry, polish slowly
53.1.7 Lubricate the ground-glass joint with silicone grease. to avoid overheating. Do not use abrasives with grinding aids;
53.1.8 Cover the flask with the condenser and circulate some grinding aids contain fluorides that can affect the
cooling water. measured corrosion rate.
53.1.9 Heat the solution slowly until all of the copper sulfate 55.4 Remove all traces of oxide scale and heat tint formed
is dissolved. during heat treatments. Any scale that cannot be removed by
53.1.10 (Warning—It has been reported that violent boiling grinding (for example, in stamped numbers) may be removed
resulting in acid spills can occur. It is important to ensure that by using one of the pickling solutions described in Practice
the concentration of acid does not increase and that an adequate A380/A380M, Table A1.1. (Residual oxide scale causes gal-
number of boiling chips (which are resistant to attack by the vanic action and consequent activation in the test solution.)
test solution) are present.)
55.5 Measure the specimens, including the inner surfaces of
54. Sampling any holes, to the nearest 0.05 mm (0.001 in.) and calculate the
54.1 Obtain and prepare only base metal samples. total exposed area.
54.1.1 There are two classes of specimens to be considered: 55.6 Degrease the specimens using suitable nonchlorinated
base metal, and process-affected metal. Process-affected metal agents, such as soap and lukewarm water, or acetone. Dry the
contains any condition that affects the corrosion properties of specimens and weigh each one to the nearest 0.001 g. Store the
the material in a non-uniform way, such as (but not limited to) specimens in a desiccator until the test is to be performed.
welds; carburized, nitrided, or oxidized surfaces; mechanical
deformation; and areas affected by heat. Base metal has none 56. Procedure
of these conditions. 56.1 If the test solution is not already boiling, bring it to
54.1.2 The Practice F test involves immersing the entire boiling.
specimen and averaging the mass loss over the entire surface of
56.1.1 Keep the flask covered with the condenser (with
the specimen. Welding, carburization, mechanical deformation,
cooling water flowing) except when inserting or removing
and the like, affect only part of a specimen.
specimens. (See Note 7.)
54.1.3 The mass loss rate from process-affected metal is
expected to differ from that from base metal; the presence of 56.2 Turn off the heat source and allow the boiling to
process-affected metal in a specimen will affect the calculated subside.
test result in an unpredictable way. 56.3 Place the specimen in a second glass cradle.
54.1.4 If the presence of these or other localized conditions
is a concern to the purchaser, then tests that do not average the 56.4 Uncover the flask.
mass loss over the total specimen surface area, such as Practice 56.5 Insert the specimens.

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 A262 − 15 (2021)
56.6 Replace the condenser immediately, restore cooling 56.11 Changes to the solution during the 120-h test period
water flow, and turn on the heat source. are not necessary.
56.7 Mark the liquid level on the flask to provide a check on 57. Calculation and Report
vapor loss, which would result in concentration of the acid. If 57.1 The effect of the acid solution on the material is
there is an appreciable change in the level, repeat the test with measured by determining the loss of weight of the specimen.
fresh solution and a reground specimen. The corrosion rate should be reported as millimetres of
penetration per month (Note 9) calculated using Eq 1.
56.8 Continue immersion of the specimen for 120 h, then
remove the specimen, rinse in water and acetone, and dry. If 58. Precision and Bias
any adherent copper remains on the specimen, it may be 58.1 Precision—The precision of Practice F is being deter-
removed by a brief immersion in concentrated nitric acid at mined.
room temperature.
58.2 Bias—This practice has no bias because the resistance
56.9 Weigh the specimen and subtract the weight from the to intergranular corrosion is defined only in terms of this
original weight. practice.
56.10 Intermediate weighings are usually not necessary; the 59. Keywords
test can be run without interruption. However, if preliminary 59.1 austenitic stainless steel; copper sulfate; corrosion
results are desired, the specimen can be removed at any time testing; etch structures; ferric sulfate; intergranular corrosion;
for weighing. nitric acid; oxalic acid

APPENDIX

Nonmandatory Information

X1. APPLICATION OF THESE TEST METHODS

X1.1 General alloys. Such sigma phase may or may not be visible in the
X1.1.1 These test methods detect one or more of three microstructure depending on the etching technique and mag-
types of susceptibility to intergranular attack: chromium nification used. Not all of the test methods can detect sigma
carbide, sigma phase, and end-grain. The choice of test method phase; see the discussions below.
is affected by the intended service, the type or types of attack X1.1.5 In most cases either the 15-h copper–copper sul-
expected from that service, and the grade of material to be fate–16 % sulfuric acid test or the 120-h ferric sulfate-sulfuric
evaluated.
acid test, combined with the Oxalic Acid Etch Test, will
X1.1.2 These practices describe the procedures by which provide the required information in the shortest time. All
the tests are conducted to determine the susceptibility of stainless grades listed in this appendix may be evaluated in
austenitic stainless steels to intergranular attack. The presence these combinations of screening and corrosion tests, except
or absence of intergranular corrosion in these tests is not those specimens of molybdenum-bearing grades (for example
necessarily a measure of the performance of the material in 316, 316L, 317, and 317L), which represent steel intended for
other corrosive media. The tests do not provide a basis for use in nitric acid environments.
predicting resistance to other forms of corrosion, such as
general corrosion, pitting, or stress-corrosion cracking. X1.1.6 The 240-h nitric acid test should be applied to
X1.1.3 Susceptibility to intergranular attack associated with stabilized and molybdenum-bearing grades intended for ser-
the precipitation of chromium carbides is readily detected in all vice in nitric acid and to all stainless steel grades that might be
five tests. subject to end grain corrosion in nitric acid service.
X1.1.4 Sigma phase may be present in wrought chromium- X1.1.7 Extensive test results on various types of stainless
nickel-molybdenum steels, in titanium-or columbium- steels evaluated by these practices have been published in
stabilized alloys, and in cast molybdenum-bearing stainless Ref. (8).

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 A262 − 15 (2021)

PRACTICE A—OXALIC ACID ETCH TEST

X1.2 The Oxalic Acid Etch Test is used for acceptance of while giving unacceptable results in the hot acid test. In the
material but not for rejection of material. This may be used in latter case the etch test would pass material that should have
connection with other evaluation tests to provide a rapid been rejected.
method for identifying those specimens that are certain to be
free of susceptibility to rapid intergranular attack in these other X1.2.3 When listed, the etch test can reduce the time
tests. required to determine whether the material represented by the
specimen will have a low corrosion rate in that hot acid test.
X1.2.1 The etch test is suitable for use only when it is listed However, when the etch test shows a suspect structure, the
in the applicable table under the specified hot acid test. specified hot acid must be performed to avoid rejecting good
X1.2.2 Grades not listed in the applicable table either have material.
not been evaluated for use of Practice A with that hot acid test,
or have been found to give acceptable results in the etch test

PRACTICE B—FERRIC SULFATE-SULFURIC ACID TEST

X1.3 Practice B—Ferric sulfate-sulfuric acid test is a 120-h X1.3.3 The ferric sulfate-sulfuric acid test does not detect
test in boiling solution. susceptibility to intergranular attack associated primarily with
sigma phase in wrought chromium-nickel-molybdenum stain-
X1.3.1 The ferric sulfate-sulfuric acid test may be used to
less steels (316, 316L, 317, 317L), which is known to lead to
evaluate the heat treatment accorded as-received material. It
rapid intergranular attack in certain nitric acid environments. It
may also be used to check the effectiveness of stabilizing
does not detect susceptibility to end grain attack, which is also
columbium or titanium additions and of reductions in carbon
found in certain nitric acid environments.
content in preventing susceptibility to rapid intergranular
attack. It may be applied to wrought products (including tubes), NOTE X1.1—To detect susceptibility to intergranular attack associated
with sigma phase in austenitic stainless steels containing molybdenum, the
castings, and weld metal. nitric acid test, Practice C, should be used.
X1.3.2 The ferric sulfate-sulfuric acid test detects suscepti- X1.3.4 The Oxalic Acid Etch Test (Practice A) may be used
bility to intergranular attack associated primarily with chro- to screen certain grades from testing in the ferric sulfate-
mium carbide precipitate in the unstabilized austenitic stainless sulfuric acid test; see Table 1. Grades not listed in Table 1
steels 304, 304L, 316, 316L, 317, 317L, CF-3, CF-8, CF3M, either have not been evaluated for use of Practice A with the
CF8M, CG3M, and CG8M; to intergranular attack associated ferric sulfate-sulfuric acid test or have been found to give
with sigma phase in 321, 347, CF-3M, CF-8M, CG3M, and acceptable results in the etch test while giving unacceptable
CG8M. It also reveals susceptibility associated with a sigma- results in the ferric sulfate–sulfuric acid test, thus passing
like phase constituent in stabilized stainless steels 321 and 347, material that should be rejected.
and in cast chromium-nickel-molybdenum stainless steels
CF-3M, CF-8M, CG-3M, and CG-8M.

PRACTICE C—NITRIC ACID TEST

X1.4 Practice C—Nitric test is a 240-h test in boiling for extra-low-carbon molybdenum-bearing grades unless the
solution. material tested is to be used in nitric acid service.
X1.4.1 The boiling nitric acid test may be used to evaluate X1.4.3 The Practice C test detects susceptibility to rapid
the heat treatment accorded “as-received” material. It is also intergranular attack associated with chromium carbide precipi-
sometimes used to check the effectiveness of stabilizing tate and with sigma-like phase precipitate. The latter may be
elements and of reductions in carbon content in preventing formed in molybdenum-bearing and in stabilized grades of
susceptibility to rapid intergranular attack. This practice may austenitic stainless steels and may or may not be visible in the
be applied to wrought products (including tubes), castings, and microstructure. This test also reveals susceptibility to end grain
weld metal of the various grades of stainless steel attack in all grades of stainless steels.
X1.4.2 Intergranular attack in nitric acid is associated with X1.4.4 The nitric acid test detects susceptibility to inter-
one or more of the following: intergranular precipitation of granular attack associated primarily with chromium carbide
chromium carbides, sigma or transition phases in precipitate in 304, 304L, 316, 316L, 317, 317L, 321, 347,
molybdenum-bearing grades, and sigma phase constituents in CF-3, CF-8, CF-3M, and CF-8M; to intergranular attack
stabilized grades. The boiling nitric acid test should not be used associated with sigma phase in 316, 316L, 317, 317L, 321,

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 A262 − 15 (2021)
347, CF-3M, and CF-8M; and to end-grain attack in 304, 304L, been found to give acceptable results in the etch test while
316, 316L, 317, 317L, 321, and 347. The nitric acid test may giving unacceptable results in the nitric acid test, thus passing
be also applied to 309, 310, 348, 410, 430, 446, and CN-7M. material that should be rejected. Specifically, grades 316, 316L,
Those grades in which sigma phase may form must be tested in 317, 317L, 347, and 321 cannot be screened because these
nitric acid test when destined for service in nitric acid. steels may contain sigma phase not visible in the etch structure.
X1.4.5 The Oxalic Acid Etch Test (Practice A) may be used This may cause rapid intergranular attack in the nitric acid test.
to screen certain grades from testing in the nitric acid test; see
Table 2. Grades not listed in Table 2 either have not been
evaluated for use of Practice A with the nitric acid test or have

PRACTICE E—COPPER–COPPER SULFATE–16 % SULFURIC ACID TEST

X1.5 Practice E—Copper–Copper Sulfate–16 % Sulfuric X1.5.3 It does not detect susceptibility to intergranular
Acid Test is a 15-h test in a boiling solution with the test attack associated with sigma phase or end-grain corrosion, both
specimen embedded in metallic copper shot or grindings. After of which have been observed only in certain nitric acid
exposure in the boiling solution, the specimen is bent. environments.
X1.5.1 This test may be used to evaluate the heat treatment X1.5.4 The Oxalic Acid Etch Test (Practice A) may be used
accorded as-received material. It may also be used to evaluate to screen certain grades from testing in the copper–copper
the effectiveness of stabilizing element additions (Cb, Ti, and sulfate–16 % sulfuric acid test; see Table 4. Grades not listed in
so forth) and reductions in carbon content to aid in resisting Table 4 either have not been evaluated for use of Practice A
intergranular attack. All wrought products and weld material of with the copper–copper sulfate-16 % sulfuric acid test or have
austenitic stainless steels can be evaluated by this test. been found to give acceptable tests in the etch test while giving
X1.5.2 Practice E indicates susceptibility to intergranular unacceptable results in the copper–copper sulfate–16 % sulfu-
attack associated with the precipitation of chromium-rich ric acid test, thus passing material that should be rejected.
carbides in 201, 202, 301, 304, 304L, 316, 316L, 317, 317L,
321, and 347.

PRACTICE F—COPPER–COPPER SULFATE–50 % SULFURIC ACID TEST

X1.6 Practice F—Copper–Copper Sulfate–50 % Sulfuric X1.6.3 The Oxalic Acid Etch Test (Practice A) may be used
Acid Test is a 120-h test in a boiling solution that contains to screen certain grades from testing in the copper–copper
metallic copper. sulfate–50 % sulfuric acid test; see Table 6. Grades not listed in
X1.6.1 This test detects susceptibility to intergranular attack Table 6 either have not been evaluated for use of Practice A
associated with the precipitation of chromium-rich carbides in with the copper–copper sulfate–50 % sulfuric acid test or have
CF-3M, CF-8M, and 316Ti. been found to give acceptable results in the etch test while
giving unacceptable results in the copper–copper sulfate–50 %
X1.6.2 This test does not detect susceptibility to attack
associated with sigma phase. sulfuric acid test, thus passing material that should be rejected.

REFERENCES

(1) For original descriptions of the use of etch structure classifications, sion of Stainless Alloys, ASTM STP 656, R. F. Steigerwald ed., ASTM,
see Streicher, M. A., “Screening Stainless Steels from the 240-h Nitric 1978, pp. 3–84.
Acid Test by Electrolytic Etching in Oxalic Acid,” ASTM Bulletin, No. (4) The use of copper to accelerate the intergranular corrosion of
188, February 1953, p. 35; also “Results of Cooperative Testing sensitized austenitic stainless steels in copper sulfate–sulfuric acid
Program for the Evaluation of the Oxalic Acid Etch Test,” ASTM was first described by H. J. Rocha in the discussion of a paper by
Bulletin, No. 195, January 1954, p. 63. Brauns, E., and Pier, G., Stahl und Eisen, Vol 75, 1955, p. 579.
(2) For original descriptions of the boiling nitric acid test, see Huey, W. (5) For original evaluation of the copper–copper sulfate–sulfuric acid test,
R., “Corrosion Test for Research and Inspection of Alloys,” see Scharfstein, L. R., and Eisenbrown, C. M., “An Evaluation of
Transactions, American Society of Steel Treating, Vol 18 , 1930, p. Accelerated Strauss Testing,” ASTM STP 369, ASTM, 1963, pp.
1126; also, “Report of Subcommittee IV on Methods of Corrosion 235–239.
Testing,” Proceedings, ASTM, Vol 33, Part I, 1933, p. 187. (6) Subtle effects due to variations in copper surface areas, galvanic
(3) Streicher, M. A.,“Theory and Application of Evaluation Tests for contact, condenser design, etc., are described by Herbsleb, G., and
Detecting Susceptibility to Intergranular Attack in Stainless Steels and Schwenk, W., “Untersuchungen zur Einstellung des Redoxpotentials
Related Alloys-Problems and Opportunities,” Intergranular Corro- der Strausschen Lösung mit Zusatz von Mettalischem Kupfer,”

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 A262 − 15 (2021)
Corrosion Science, Vol 7, 1967, pp. 501–511. ed., ASTM, 1978, pp. 146–153.
(7) Walker, W. L., “Variations in the Evaluation of ASTM A262, Practice (8) Brown, M. H., “Behavior of Austenitic Stainless Steels in Evaluation
E, Results(ASTM Subcommittee A01.14 Round Robin),” Intergranu- Tests for the Detection of Susceptibility to Intergranular Corrosion,”
lar Corrosion of Stainless Alloys, ASTM STP 656, R. F. Steigerwald Corrosion, Vol. 30, January 1974, pp. 1–12.

BIBLIOGRAPHY

(1) For original description of ferric sulfate-sulfuric acid test, see (3) See Industrial and Engineering Chemistry, Vol 17, 1925, p. 756;
Streicher, M. A., “Intergranular Corrosion Resistance of Austenitic also, “A.C.S. Analytical Reagents. Specifications Recommended by
Stainless Steels: A Ferric Sulfate-Sulfuric Acid Test,” ASTM Bulletin, Committee on Analytical Reagents,” American Chemical Society,
No. 229, April 1958, pp. 77–86. March 1941.
(2) For details, see DeLong, W. B.,“Testing Multiple Specimens of
Stainless Steels in a Modified Boiling Nitric Acid Test Apparatus,”
Symposium on Evaluation Tests for Stainless Steels, ASTM STP 93,
ASTM, 1950, p. 211.

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