Designation: G36 − 94 (Reapproved 2013)

Standard Practice for

Evaluating Stress-Corrosion-Cracking Resistance of Metals
and Alloys in a Boiling Magnesium Chloride Solution 1
This standard is issued under the fixed designation G36; 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 priate safety and health practices and determine the applica-
1.1 This practice describes a procedure for conducting bility of regulatory limitations prior to use. See Section 7 for
stress-corrosion cracking tests in a boiling magnesium chloride specific safety precautions.
solution. Although this test may be performed using various 2. Referenced Documents
concentrations of magnesium chloride, this procedure covers a
2.1 ASTM Standards:5
test solution held at a constant boiling temperature of 155.0 6
D1193 Specification for Reagent Water
1.0°C (311.0 6 1.8°F). The boiling points of aqueous magne-
G1 Practice for Preparing, Cleaning, and Evaluating Corro-
sium chloride solutions at one atmosphere pressure as a
sion Test Specimens
function of concentration are shown graphically in Fig. 1.2 A
G15 Terminology Relating to Corrosion and Corrosion Test-
suggested test apparatus capable of maintaining solution con-
ing (Withdrawn 2010)6
centration and temperature within the prescribed limits for
G30 Practice for Making and Using U-Bend Stress-
extended periods of time is also described herein.3
Corrosion Test Specimens
1.2 The boiling magnesium chloride test is applicable to
wrought, cast, and welded stainless steels and related alloys. It 3. Terminology
is a method for detecting the effects of composition, heat 3.1 Definitions—For definitions of terms used in this prac-
treatment, surface finish, microstructure, and stress on the tice see Terminology G15.
susceptibility of these materials to chloride stress corrosion
cracking.4 4. Summary of Practice
1.3 This practice is concerned primarily with the test 4.1 A predetermined quantity of reagent grade magnesium
solution, which may be used with a variety of stress corrosion chloride and some distilled water are added to a container. The
test specimens, surface finishes, and methods of applying container and contents, with thermometer and condenser
stress. affixed, are placed on a source of heat. When the magnesium
chloride solution boils, it is adjusted to maintain the desired
1.4 This standard does not purport to address all of the concentration and boiling point through the addition of small
safety concerns, if any, associated with its use. It is the quantities of either water or salt.
responsibility of the user of this standard to establish appro-
4.2 After the solution has stabilized at the desired boiling
point for the test, the stressed specimens are added. Depending
1
This practice is under the jurisdiction of ASTM Committee G01 on Corrosion upon the intent of the test, the specimens should be given
of Metals and is the direct responsibility of Subcommittee G01.06 on Environmen-
tally Assisted Cracking.
periodic inspections. If the duration of test exceeds 7 days, the
Current edition approved May 1, 2013. Published July 2013. Originally approved solution should either be changed or the suggested or similar
in 1973. Last previous edition approved in 2006 as G36 – 94 (2006). DOI: test apparatus used.
10.1520/G0036-94R13.
2
Available data on the relationship of concentrations and boiling points of 5. Significance and Use
magnesium chloride solutions are critically reviewed and supplemented by I. B.
Casale in “Boiling Points of Magnesium Chloride Solutions—Their Application in 5.1 For most applications, this environment provides an
Stress Corrosion Studies,” Corrosion , Vol 23, 1967, pp. 314–17. accelerated method of ranking the relative degree of stress-
3
The apparatus and test procedures for maintaining constant boiling tempera- corrosion cracking susceptibility for stainless steels and related
tures of magnesium chloride solutions for stress corrosion tests are described by M.
A. Streicher and A. J. Sweet in Corrosion, Vol 25, 1969, pp. 1–6.
4 5
The use of concentrated magnesium chloride solutions for determining the For referenced ASTM standards, visit the ASTM website, www.astm.org, or
susceptibility to stress corrosion cracking of austenitic and ferritic stainless steels contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
and related nickel-base alloys was first described by M. A. Scheil, Symposium on Standards volume information, refer to the standard’s Document Summary page on
Stress Corrosion Cracking of Metals, ASTM STP 64, ASTM, 1945, p. 395. the ASTM website.
6
(Although currently out of print, copies may be obtained from University Micro- The last approved version of this historical standard is referenced on
films, Inc., 300 North Zeeb Rd., Ann Arbor, MI 48106.) www.astm.org.

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 G36 − 94 (2013)
stress corrosion cracking. A suggested apparatus, shown in Fig.
X1.1, meets these requirements. Design details of this appara-
tus are given in Appendix X1.

7. Reagents
7.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society,
where such specifications are available.7 Other grades may be
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
7.2 Purity of Water—Reagent water Type IV (Specification
D1193) shall be used to prepare the test solutions.
7.3 Magnesium Chloride(MgCl2·6H2O)—A solution of
magnesium chloride that boils at 155.0 6 1.0°C (311.0 6
1.8°F) is used in this test. A second 25 weight percent solution
of magnesium chloride is required for the trap if the test
duration exceeds seven days without a solution change and the
suggested apparatus is used.
7.3.1 To prepare about 400 mL of the test solution for use in
a 1-L Erlenmeyer flask or other container, weigh 600 g of
reagent grade MgCl2·6H2O and add this to the flask containing
FIG. 1 Boiling Points of Aqueous Magnesium Chloride Solutions a thermometer along with 15 mL of reagent water.
at One Atmosphere as a Function of Concentration2
7.3.2 Add 10 to 15 boiling chips or other boiling aids.
7.3.3 Heat by placing the flask on a hot plate or other
alloys in aqueous chloride-containing environments. Materials suitable source of heat and put the condenser in place, leaving
that normally provide acceptable resistance in hot chloride off the trap. Hook up the cooling water supply to the condenser.
service may crack in this test. The test may not be relevant to 7.3.4 When the solution boils vigorously and there is no
stress-corrosion cracking in polythionic acid or caustic envi- more dripping of condensate, slowly add small quantities (4 to
ronments. 5 mL) of reagent water at the top of the condenser to reduce the
temperature to 155.0°C (311.0°F). Use extreme caution when
5.2 Resistance to stress-corrosion cracking in boiling mag-
adding the water to the boiling magnesium chloride solution.
nesium chloride (155.0°C (311.0°F)) should, where possible,
Cool water can form a layer on top of the magnesium chloride,
be correlated to resistance in service for the materials of
and when it reaches the bottom of the flask, bumping can occur.
interest. However, such correlations may not always be pos-
Use a protective shield.
sible.
NOTE 1—If too much water has been added, add some crystals of
5.3 Boiling magnesium chloride may also cause pitting of MgCl2·6H2O through the condenser until a temperature of 155.0°C
many stainless alloys. This leads to the possibility of confusing (311.0°F) is attained.
stress-corrosion failures with mechanical failures induced by
7.4 To prepare the 25 weight percent solution for the trap
corrosion-reduced net cross sections. This danger is particu-
(Fig. X1.3), place 53.4 g of MgCl2·6H2O and 46.6 mL of
larly great when small cross section samples, high applied
reagent water in a flask and allow the crystals to dissolve at
stress levels, long exposure periods, stress-corrosion resistant
room temperature.
alloys, or a combination thereof are being used. Careful
examination is recommended for correct diagnosis of the cause 8. Safety Precautions
of failure.
8.1 When cold, magnesium chloride can be handled with
6. Apparatus the minimum protective equipment of rubber gloves and
goggles. Maximum protective measures should be taken to
6.1 Any inert, transparent apparatus with provisions for a
prevent boiling magnesium chloride from coming into contact
thermometer and water-cooled condenser can be used, pro-
with the skin. Severe burns can result as the hot magnesium
vided that it has been designed to contain the stressed specimen
while maintaining a constant temperature and concentration of
the magnesium chloride solution by minimizing or preventing 7
Reagent Chemicals, American Chemical Society Specifications , American
losses of condensate and water vapor during prolonged periods Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
of test. Small losses of water from a solution of magnesium
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
chloride will lead to large increases in the boiling point of the and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
solution with a reduction in the time to failure of a specimen by MD.
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 G36 − 94 (2013)
chloride adheres to the skin forming a crust which causes deep rods or tubes. The design for two types of test specimens that
burns. The severity of the burns can be reduced by taking can be used with the suggested apparatus can be found in
proper and immediate first aid measures and by contacting a footnote 3.
physician.
10. Procedure
8.1.1 In the advent of a spill or accident, the hot magnesium
chloride should be quickly flushed from the skin with large 10.1 Collect the apparatus and test specimens in preparation
quantities of cold water to minimize the burning, followed by for the test. If the suggested test apparatus is used, assemble as
immediate first aid and medical attention. outlined in Appendix X1.
8.1.2 All heating or boiling of magnesium chloride should 10.2 Prepare the test solution by adding a known quantity of
be done in a shielded area with protection by hood or shield, or reagent grade MgCl2·6H2O, reagent water, and some boiling
both. aids to the container fitted with a thermometer and water-
8.1.3 Minimum personal protective equipment for handling cooled condenser. After applying heat, adjust the concentration
boiling magnesium chloride should include safety glasses or of the solution by slowly adding small quantities (4 to 5 mL)
goggles, face shield, laboratory coat, and rubber gloves with of distilled water until the solution reaches the constant-boiling
cotton inner gloves. temperature of 155 6 1.0°C (311.0 6 1.8°F). Now place the
8.1.4 Disposal of the magnesium chloride should be accom- previously prepared test specimens in the container.
plished in accordance with the material safety data supplied
with the chemical or by the chemical manufacturer or supplier. 11. Report
8.1.5 Do not remelt the solidified magnesium chloride. 11.1 Record starting time, type of specimen, stress, and type
Localized melting adjacent to the heat source and below the exposure. A clear distinction must be made in the type of
solid layer of magnesium chloride can cause sufficient stresses exposure; that is, complete immersion, vapor phase exposure,
through volume expansion to crack the containing vessel. or a combination of immersion and exposure to the vapor
phase. The time required to initiate cracks, the rate of crack
9. Test Specimens growth, and the time to failure may be of importance, depend-
ing upon the purpose of the test.
9.1 Any type of stress corrosion test specimen can be used
11.1.1 Periodic removal of the specimen from the solution
with this test solution.8 See Practice G1 and G30.
may be necessary to determine the time when cracks first
9.2 The test specimen must be thick enough so that the appear and the rate of crack propagation. Microscopic exami-
applied stress does not cause mechanical rupture when the nation of polished surfaces is required to detect crack initiation.
cross section is reduced by pitting or general corrosion. All stressed surfaces should be examined at magnifications up
9.3 Whenever possible, only one specimen should be tested to 20×. Metallographic examination of exposed surfaces and of
in each flask. If more than one specimen is tested in a flask, the polished and etched cross sections at higher magnifications are
specimens should be of the same alloy in order to avoid the necessary at the end of the test to establish the type of cracking:
possible deleterious effects of the corrosion products of one transgranular, intergranular, or mixed.
alloy on the performance of the other alloy. 11.1.2 Ruptured specimens should also be examined for
evidence of mechanical failure resulting from the action of
9.4 The test specimens must be kept from direct contact
applied stress on specimens whose cross sections have been
with heated surfaces by glass supports. Metal specimen holders
reduced by general or pitting corrosion, or both. Such failures
used for stressing specimens should also be supported on glass
usually show evidence of ductility. Duplicate tests with thicker
specimens should be made in case of doubt.
8
For a comprehensive discussion of the various types of test specimens 12. Keywords
available, see “Stress Corrosion Testing Methods,” Stress Corrosion Testing, ASTM
STP 425, ASTM. (Although currently out of print, copies may be obtained from
12.1 accelerated test; apparatus; boiling magnesium chlo-
University Microfilms, Inc., 300 North Zeeb Rd., Ann Arbor, MI 48106.) See also ride; glassware; nickel containing alloy; stainless steels; stress-
Section 2 of this practice. corrosion cracking

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 G36 − 94 (2013)
APPENDIX

(Nonmandatory Information)

X1. TEST APPARATUS

X1.1 The following test apparatus is suggested for its ability NOTE X1.4—Use of a thermometer with a ground-glass inner joint in
to maintain a constant temperature and solution concentration place of the adapter results in appreciable loss of water vapor at this hot
joint.
over a long period of time. Use of this apparatus is not
mandatory and is presented here only as a guide. X1.2.6 When assembling the above components, do not use
any lubricants on any of the ground-glass joints.
X1.2 The suggested test apparatus is shown in Fig. X1.1 and
the design details are given below: X1.3 Assembly:
X1.2.1 Flask—the 1-L Erlenmeyer flask (Fig. X1.2) has a X1.3.1 The thermometer along with its adapter is inserted
ground-glass 45/50 outer joint at the mouth and a 10/30 into the side arm of the Erlenmeyer flask and positioned so that
ground-glass outer joint to hold the thermometer. the bulb is located about 7.5 mm (5⁄16 in.) from the bottom of
the flask. The adapter is tightened to prevent the loss of water
NOTE X1.1—Other flasks or containers may be used. For tests requiring
a larger container, a 3-L round bottom flask with a 71/60 ground-glass during the test and the MgCl2·6H2O, reagent water, and boiling
outer joint can also be used. The height of the condenser (X1.2.2) and the aids are added to the flask. After positioning the water-cooled
dimensions of the trap (Fig. X1.3) can be the same as for the 1-L condenser on top of the flask, the whole assembly is placed on
Erlenmeyer flask. a hot plate or other suitable source of heat. Do not attach the
X1.2.2 Condenser (Fig. X1.4)—a modified Allihn con- trap at this time.
denser with a 45/50 ground-glass inner joint. In place of the X1.3.2 The solution concentration is adjusted by slowly
drip tip on the conventional condenser, the exit must be formed adding small portions (4 to 5 mL) of reagent water until the
as shown in Fig. X1.4. A smooth exit on the condenser is constant boiling temperature of 155 6 1°C (311.0 6 1.8°F) is
essential to prevent dripping. The water jacket of the condenser attained. The previously prepared test specimens and holder
should be at least 250 mm long. At the top of the condenser, a are now ready to be placed in the flask. This is accomplished
29/26 ground-glass outer joint is required to hold the trap in by removing the condenser from the flask, immersing the
place. specimen and specimen holder in the boiling solution (with
NOTE X1.2—Dripping of condensate into hot magnesium chloride caution), and quickly replacing the condenser.
solution from the “drip tip” of a conventional Allihn condenser results in
a pulsating generation of water vapor. These pressure waves lead to the X1.3.3 Cut a 50 by 450-mm (2 by 18-in.) strip of commer-
loss of water vapor at the top of the condenser. Initially, there may be some cial aluminum foil. Wrap this foil around the outside of the
dripping from the condenser until there is complete wetting of the walls of joint between the condenser and the flask and press the foil
the flask by the condensate. against the glass so that the joint is well covered and none of
X1.2.3 Trap—containing a 25 weight percent solution of the foil is in contact with the hot flask below the joint.
magnesium chloride (Fig. X1.3), and affixed to the top of the
NOTE X1.5—The purpose of the aluminum foil is to prevent loss of
condenser to eliminate vapor losses by diffusion during tests in condensate by evaporation where the top of the ground-glass surface of
excess of 7 days. The trap is joined to the condenser by a 29/26 the joint is exposed to the air. Condensate rises by capillary action in the
ground glass inner joint. joint and evaporates in the warm air.
X1.2.4 Thermometer— required to adjust the boiling point, X1.3.4 If the period of exposure exceeds 7 days, a liquid
and thereby the concentration of the magnesium chloride trap is required at the top of the condenser to maintain the
solution when it is prepared, and to monitor the solution constant boiling point of 155.0 6 1.0°C (311.0 6 1.8°F)
temperature throughout the test. The graduations must clearly without new additions of water to the boiling MgCl2 solution.
show 1°C increments in the range of 130 to 170°C (266 to Fill the trap to the liquid level line with a 25% solution of
338°F). When the specially designed thermometer of Fig. X1.5 MgCl2 (see 7.4). As soon as the condensate stops dripping
is used in the 1-L Erlenmeyer flask of Fig. X1.2, no more space from the condenser and flows down the wall of the Erlenmeyer
is needed on hot plates than that taken up by the flasks flask in a continuous stream, place the trap on top of the
themselves. A modified ASTM Thermometer 86D with a condenser.
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temperature range from 95 to 170°C (203 to 338°F) in 1°C

NOTE X1.6—Whenever the trap is needed, it must be used with the
subdivisions can also be used with this apparatus. modified condenser because the pressure pulses generated by “drip tip”
condensers exceed the capacity of the trap to absorb sudden changes in
NOTE X1.3—The thermometer should be checked for the presence of
pressure within the flask.
gas bubbles before each use. These can be removed by cooling the lower
part of the bulb (dry ice) and gently tapping the thermometer. Storage of X1.3.5 During long-time tests, there may be a slow drop in
a thermometer in a vertical position will prevent appearance of bubbles. the level of liquid in the trap because of evaporation of water
X1.2.5 Adapter—a fluorocarbon resin adapter containing a at the top of the trap from the 25 % MgCl2 solution. This level
rubber O-ring seal for a 10/30 ground-glass outer joint must be should be brought up to the liquid level line by additions of
used to hold the thermometer in place in the flask. reagent water every 7 to 14 days.

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FIG. X1.1 Assembly of Glass Apparatus for Stress-Corrosion Test in Boiling Magnesium Chloride with U-Bend Specimen in Place
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 G36 − 94 (2013)

FIG. X1.2 Modified Erlenmeyer Flask (1000 mL)

FIG. X1.4 Modification of Allihn Condenser to Prevent Loss of

Vapor

FIG. X1.3 Trap for Top of Condenser to Prevent Loss of Vapor

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FIG. X1.5 Design of Thermometer for Use in Flask of Fig. X1.2

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