Designation: G35 – 98 (Reapproved 2010)

Standard Practice for

Determining the Susceptibility of Stainless Steels and
Related Nickel-Chromium-Iron Alloys to Stress-Corrosion
Cracking in Polythionic Acids1
This standard is issued under the fixed designation G35; 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.

1. Scope G1 Practice for Preparing, Cleaning, and Evaluating Corro-

1.1 This practice covers procedures for preparing and con- sion Test Specimens
ducting the polythionic acid test at room temperature, 22 to G15 Terminology Relating to Corrosion and Corrosion
25°C (72 to 77°F), to determine the relative susceptibility of Testing3
stainless steels or other related materials (nickel-chromiumiron G30 Practice for Making and Using U-Bend Stress-
alloys) to intergranular stress corrosion cracking. Corrosion Test Specimens
1.2 This practice can be used to evaluate stainless steels or 3. Summary of Practice
other materials in the “as received” condition or after being
subjected to high-temperature service, 482 to 815°C (900 to 3.1 The stressed specimens are placed in the container along
1500°F), for prolonged periods of time. with a sensitized and stressed AISI Type 302 (UNS S30200) or
1.3 This practice can be applied to wrought products, Type 304 (UNS S30400) stainless steel control specimen. A
castings, and weld metal of stainless steels or other related sufficient amount of the previously prepared polythionic acid
materials to be used in environments containing sulfur or solution is added to the container to immerse the test speci-
sulfides. Other materials capable of being sensitized can also mens. A cover is placed on the container and the test is carried
be tested in accordance with this test. out at room temperature.
1.4 This practice may be used with a variety of stress 4. Significance and Use
corrosion test specimens, surface finishes, and methods of
applying stress. 4.1 This environment provides a way of evaluating the
1.5 This standard does not purport to address all of the resistance of stainless steels and related alloys to intergranular
safety concerns, if any, associated with its use. It is the stress corrosion cracking. Failure is accelerated by the presence
responsibility of the user of this standard to establish appro- of increasing amounts of intergranular precipitate. Results for
priate safety and health practices and determine the applica- the polythionic acid test have not been correlated exactly with
bility of regulatory limitations prior to use. For more specific those of intergranular corrosion tests. Also, this test may not be
precautionary statements, see Section 7. relevant to stress corrosion cracking in chlorides or caustic
environments.
2. Referenced Documents 4.2 The polythionic acid environment may produce areas of
2.1 ASTM Standards:2 shallow intergranular attack in addition to the more localized
D1193 Specification for Reagent Water and deeper cracking mode of attack. Examination of failed
specimens is necessary to confirm that failure occurred by
cracking rather than mechanical failure of reduced sections.
1
This practice is under the jurisdiction of ASTM Committee G01 on Corrosion 5. Apparatus
of Metals and is the direct responsibility of Subcommittee G01.06 on Environmen-
tally Assisted Cracking.
5.1 Any suitable glass or other transparent, inert container
Current edition approved Sept. 1, 2010. Published November 2010. Originally can be used to contain the acid solution and stressed specimens
approved in 1988. Last previous edition approved in 2004 as G35–98(2004). DOI: during the period of test at room temperature, 22 to 25°C (72
10.1520/G0035-98R10.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Withdrawn. The last approved version of this historical standard is referenced
the ASTM website. on www.astm.org.

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

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 G35 – 98 (2010)
to 77°F). The container should be fitted with a removable top 8. Test Specimens
to reduce evaporation and to allow access to the stressed
8.1 Any type of stress corrosion test specimen can be used
specimen (or specimens) for the periodic inspection.
with this test solution. For a comprehensive discussion of the
6. Reagents various types of test specimens available, see Ref (7), as well
6.1 Purity of Reagents—The polythionic acid solution shall as Practices G1 and G30, and Terminology G15.
be prepared using reagent grade sulfurous acid and technical 8.2 The AISI Type 302 control specimens should be sensi-
grade hydrogen sulfide; or, distilled water, commercial grade tized by heating in a furnace for 4 h at 650°C (1200°F) and
sulfur dioxide, and technical grade hydrogen sulfide. then allowing to air cool. The AISI Type 304 control specimens
6.2 Purity of Water—Reagent water Type IV (Specification should be sensitized by heating in a furnace for 2 h at 677°C
D1193) shall be used to prepare the test solutions. (1250°F) and then allowing to air cool.
6.3 Wackenroder’s or Polythionic Acid Solution (1)4—A
slow current of hydrogen sulfide is passed for an hour through 9. Procedure
a fritted glass tube into a flask containing chilled (0°C, 32°F)
9.1 Prepare the polythionic acid test solution as described in
6 % sulfurous acid, after which the liquid is kept in the
6.3 and 6.3.1.
stoppered flask for 48 h at room temperature. This operation is
repeated until the liquid no longer gives off the odor of sulfur 9.2 Prior to usage, filter the acid solution to remove the
dioxide after standing at room temperature for a few hours. excess sulfur and test for the presence of polythionic acids. The
Note safety precautions in Section 7. simplest method of testing for the acid is to expose a stressed
6.3.1 In an alternative method (2), the polythionic acid specimen of sensitized AISI Type 302 or Type 304 stainless
solution is prepared by passing a slow current of sulfur dioxide steel. The specimen should fail by cracking in less than 1 h.
gas through a fritted glass bubbler submerged in a container of 9.3 Place the stressed specimens in the container along with
distilled water. This is continued until the solution becomes the sensitized and stressed AISI Type 302 or Type 304 stainless
saturated and then the hydrogen sulfide gas is slowly bubbled steel control sample. Add a sufficient amount of polythionic
into the sulfurous acid solution. acid solution to the container to immerse the test specimens.
6.3.2 The presence of polythionic acids in the solution Close the container and carry out the test at room temperature.
prepared in accordance with 6.3 or 6.3.1 can be checked by Record starting time for the test.
either of the following methods. Polarography (3) can be
employed to identify the thionic acids, or the percent of acid 10. Report
present in the solution can be determined by wet techniques
(4). The simplest method of checking the solution for poly- 10.1 Record starting time, type of specimen, stress, and type
thionic acids is to expose a stressed and sensitized sample of of exposure. A distinction must be made in the type of
AISI Type 302 stainless steel. The sample should fail by exposure; that is, complete immersion, vapor phase exposure,
cracking in less than 1 h. Alternatively, Type 304 sheet (0.07 % or a combination of immersion and vapor phase. The time
carbon) which has been sensitized and exposed as a U-bend required to initiate cracks, the rate of crack growth, and time to
should crack in 1 h (5). Detection of cracks can be facilitated failure may be of importance, depending upon the purpose of
by closing the legs of the U-bend and examining with a 203 the test.
binocular microscope. 10.1.1 Periodic removal of specimens from the solution
may be necessary to determine the time when cracks first
7. Safety Precautions
appear and the rate of crack propagation. Microscopical
7.1 Hydrogen sulfide should be handled with extreme cau- examination of polished surfaces is required to detect crack
tion. The characteristic odor of hydrogen sulfide cannot always initiation. All stressed surfaces should be examined at magni-
be used as an alarm system because the olfactory nerves fications up to 203 at the completion of this test. Metallo-
become deadened when exposed to a concentration of a few graphic examination of exposed surfaces and of polished and
parts per million of this gas. The maximum allowable concen- etched cross sections at higher magnifications are necessary to
tration in the air for an 8-h work day is 10 ppm, which is well establish the type of cracking.
above the level detectable by smell. Exposure to high concen-
10.1.2 Ruptured specimens should also be examined for
trations of hydrogen sulfide can be fatal. For additional
evidence of mechanical failure resulting from the action of
information on the toxicity of hydrogen sulfide, consult Ref
applied stress on specimens whose cross sections have been
(6).
7.2 Normal laboratory precautions should be observed when reduced by general or pitting corrosion or both. Such failures
handling the sulfurous or polythionic acid solutions. Hydrogen usually show evidence of ductility. Duplicate tests with thicker
sulfide should only be used in a hood observing the above specimens should be made in cases of doubt.
precautions.
11. Keywords
4
The boldface numbers in parentheses refer to a list of references at the end of 11.1 accelerated test; nickel-chromium-iron alloys; poly-
this standard. thionic acids; stainless steels; stress-corrosion cracking

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 G35 – 98 (2010)

REFERENCES

(1) Debus, H., “Chemical Investigation of Wackenroder’s Solution,” try, Vol 25, No. 2, 1953, pp. 288–290.
Journal of the Chemical Society, London, Transactions, Vol 53, 1888, (5) Crum, J. R., Adkins, M. E., and Lipscomb, W. G., “Performance of
p. 278 (paper XXV). High Nickel Alloys in Refinery and Petrochemical Environments,”
(2) Samans, C. H., “Stress Corrosion Cracking Susceptibility of Stainless Materials Performance, Vol. 25, No. 7, July, 1986, pp. 27–33.
Steels and Nickel-Base Alloys in Polythionic Acids and Acid Copper (6) Chemical Safety Data Sheet SD-36, Manufacturing Chemists Asso-
Sulfate Solution,” Corrosion, Vol 20, August 1964, pp. 256t–262t. ciation, 1825 Connecticut Ave., N.W., Washington, DC 20009.
(3) Murayama, T., “Polarography of Polythionates,” Journal of Chemical (7) “Stress Corrosion Testing Methods,” Stress Corrosion Testing, ASTM
Society of Japan, Pure Chemistry Section, Vol 74, No. 5, 1953, pp. STP 425, ASTM Testing Mats. (Out of print. Send orders directly to
349–352. University Microfilms, Inc., 300 North Zeeb Rd., Ann Arbor, MI
(4) Jay, P. R., “Determination of Polythionic Acids,” Analytical Chemis- 48106.)

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