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An American National Standard

Designation: A 923 – 01

Standard Test Methods for

Detecting Detrimental Intermetallic Phase in Wrought
Duplex Austenitic/Ferritic Stainless Steels1
This standard is issued under the fixed designation A 923; 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 (e) indicates an editorial change since the last revision or reapproval.

1. Scope to promote the formation of an intermetallic phase. In the case

1.1 The purpose of these test methods is to allow detection of common heat treatment, this region will be that which
of the presence of intermetallic phases in mill products of cooled most slowly. Except for rapidly cooled material, it may
duplex stainless steels to the extent that toughness or corrosion be necessary to sample from a location determined to be the
resistance is affected significantly. These test methods will not most slowly cooled for the material piece to be characterized.
necessarily detect losses of toughness or corrosion resistance 1.7 The tests do not determine the precise nature of the
attributable to other causes. detrimental phase but rather the presence or absence of an
1.2 Duplex (austenitic-ferritic) stainless steels are suscep- intermetallic phase to the extent that it is detrimental to the
tible to the formation of intermetallic compounds during toughness and corrosion resistance of the material.
exposures in the temperature range from approximately 600 to 1.8 An example of the correlation of thermal exposures, the
1750°F (320 to 955°C). The speed of these precipitation occurrence of intermetallic phases, and the degradation of
reactions is a function of composition and thermomechanical toughness and corrosion resistance is given in Appendix X1.
history of each individual piece. The presence of these phases 1.9 The values stated in either inch-pound or SI units are to
is detrimental to toughness and corrosion resistance. be regarded as the standard. The values given in parentheses
1.3 Correct heat treatment of duplex stainless steels can are for information only.
eliminate these detrimental phases in the mill product. Rapid 1.10 This standard does not purport to address all of the
cooling of the mill product provides the maximum resistance to safety concerns, if any, associated with its use. It is the
formation of detrimental phases by subsequent thermal expo- responsibility of the user of this standard to establish appro-
sures. priate safety and health practices and determine the applica-
1.4 Compliance with the chemical and mechanical require- bility of regulatory limitations prior to use.
ments for the applicable product specification does not neces- 2. Referenced Documents
sarily indicate the absence of detrimental phases in the mill
product. 2.1 ASTM Standards:
1.5 These test methods include the following: A 370 Test Methods and Definitions for Mechanical Testing
1.5.1 Test Method A—Sodium Hydroxide Etch Test for of Steel Products2
Classification of Etch Structures of Duplex Stainless Steels G 48 Test Methods for Pitting and Crevice Corrosion Re-
(Sections 3-7). sistance of Stainless Steels and Related Alloys by Use of
1.5.2 Test Method B—Charpy Impact Test for Classification Ferric Chloride Solution3
of Structures of Duplex Stainless Steels (Sections 8-13).
TEST METHOD A—SODIUM HYDROXIDE ETCH
1.5.3 Test Method C—Ferric Chloride Corrosion Test for
TEST FOR CLASSIFICATION OF ETCH
Classification of Structures of Duplex Stainless Steels (Sec-
STRUCTURES OF DUPLEX STAINLESS STEELS
tions 14-20).
1.6 The presence of detrimental intermetallic phases is 3. Scope
readily detected in all three tests, provided that a sample of
3.1 The sodium hydroxide etch test may be used for the
appropriate location and orientation is selected. Because the
acceptance of material but not for rejection. This test method
occurrence of intermetallic phases is a function of temperature
may be used with other evaluation tests to provide a rapid
and cooling rate, it is essential that the tests be applied to the
method for identifying those specimens that are free of
region of the material experiencing the conditions most likely
detrimental intermetallic phases as measured in these other
tests.
1
These test methods are under the jurisdiction of ASTM Committee A01 on
Steel, Stainless Steel, and Related Alloysand are the direct responsibility of
Subcommittee A01.14 on Methods of Corrosion Testing.
2
Current edition approved Sept. 10, 2001. Published October 2001. Originally Annual Book of ASTM Standards, Vol 01.03.
3
published as A 923–94. Last previous edition A 923–98. Annual Book of ASTM Standards, Vol 03.02.

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

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A 923
3.2 The sodium hydroxide etch test may be used to screen 5.2 The specimen should allow for a survey across the full
specimens intended for testing in Test Method B, Charpy thickness of the section or, in the case of a heavy section, a
Impact Test for Classification of Structures of Duplex Stainless survey from one surface through the mid-thickness of the
Steels, and in Test Method C, Ferric Chloride Corrosion Test section. The specimen shall include the mid-thickness.
for Classification of Structures of Duplex Stainless Steels. 5.3 Polishing—On all materials, cross-sectional surfaces
3.3 Reference photomicrographs are provided to show clas- should be polished to a metallographic finish suitable for
sifications of etch structures of a particular stainless steel type examination at 4003 after etching. Specimens containing
that are equivalent to acceptable or to possibly nonacceptable welds should include base metal, weld heat–affected zone, and
performance for each practice. When Test Method A is used as weld metal. The area to be etched may be prepared by grinding
a screening test for Test Method B or Test Method C, to an 80- or 120-grit finish on a grinding belt or wheel without
specimens having acceptable etch structures need not be excessive heating and then by polishing on successively finer
subjected to Test Method B or Test Method C. emery papers, No. 1, 1⁄2, 1⁄0, 2⁄0, 3⁄0, and finer. Other methods of
3.4 Table 1 indicates the applicability and acceptance crite- polishing may be acceptable.
ria for Test Method A. When Test Method A is specified as an 5.4 Etching Solution—The solution for etching is prepared
acceptance test, specimens having other than acceptable etch by adding 40 g of reagent grade sodium hydroxide (NaOH) to
structures may, at the option of the producer, be tested by Test 100 g of distilled water.
Method B or Test Method C. 5.5 Etching Conditions—The polished specimen should be
3.5 The steel shall be tested in the mill-annealed condition etched at approximately 1 to 3 V dc, for 5 to 60 s (see Note 2).
or such other conditions as are agreed upon between the NOTE 2—When etching is performed at 1 to 3 V dc with a platinum
producer and the user. cathode for 5 to 60 s, any intermetallic phase is revealed by yellow, then
brown, staining, followed by staining of the ferrite.
4. Apparatus
4.1 Source of Direct Current—Battery, generator, or recti- 5.6 Rinsing—Following etching, the specimen should be
fier capable of supplying approximately 15 V and 20 A. rinsed thoroughly in hot water and in acetone or alcohol,
4.2 Ammeter—Range from 0 to 30 A (see Note 1). followed by air drying.
4.3 Variable Resistance (see Note 1). 6. Classification of Etch Structures
4.4 Cathode—A cylindrical piece of conductive metal. 6.1 The etched surface shall be examined on a metallurgical
4.5 Large Electric Clamp, to hold the specimen to be microscope at 400 to 5003.
etched. 6.2 The etched cross-sectional areas should be examined
4.6 Metallurgical Microscope, for examination of etched thoroughly by complete traverse of the full sample and across
microstructures to 400 to 500 diameters. all zones such as weld metal, weld-affected zones, and base
4.7 Electrodes of the Etching Cell—The specimen to be metal on specimens containing welds.
etched is made the anode, and a cylindrical piece of metal as 6.3 The etch structures are classified into the following
large as the specimen to be etched is made the cathode. types:
4.8 Electrolyte, sodium hydroxide (NaOH), reagent grade. 6.3.1 Unaffected Structure (Fig. 1)—The ferrite has been
NOTE 1—The variable resistance and ammeter are placed in the circuit etched without revelation of intermetallic phase. The inter-
to measure and control the current on the specimen to be etched. phase boundaries are smooth.
6.3.2 Possibly Affected Structure (Fig. 2)—The ferrite has
5. Preparation of Test Specimens been etched with isolated indications of possible intermetallic
5.1 Examination shall be made on a longitudinal or trans- phase. The interphase boundaries may show a fine waviness.
verse section. Because high temperature or mechanical defor- 6.3.3 Affected Structure (Fig. 3)—The indications of an
mation associated with particular cutting processes may alter intermetallic phase are readily revealed before or simulta-
the structure of the steel, the cutting of the test specimen should neously with the staining of the ferrite during etching.
be by a technique that prevents these effects. Alternatively, 6.3.4 Centerline Structure (Fig. 4)—An intermetallic phase
after the specimens are cut, any material that may have been is observed as a continuous or semi-continuous phase in the
affected by high temperature or deformation associated with mid-thickness region of the product, with or without the
the cutting should be removed by machining or wet grinding affected structure outside of the mid-thickness region, indica-
prior to testing. tive of segregation.
TABLE 1 Applicability and Acceptance Criteria for 7. Interpretation and Use of the Etch Structure
Test Method A Classifications
7.1 When Test Method A is used as a screening test, the use
Grade Acceptable Nonacceptable of these etch structures depends on the test method for which
Etch Structure Etch Structure
the specimens are being screened. Important characteristics of
S31803, unaffected possibly affected
S32205, S32750 structure (Fig. 1) structure (Fig. 2) each of the test methods are described as follows.
affected structure 7.2 Test Method B—The Charpy impact test detects reduc-
(Fig. 3) tions in toughness from that of the optimal composition and
centerline structure
(Fig. 4) processing. Such reductions may be attributable to intermetal-
lic phases or to other causes not necessarily detectable by Test

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A 923

FIG. 1 Unaffected Structure in S31803: (a) Longitudinal Section FIG. 2 Possibly Affected Structure in S31803: (a) Longitudinal
and (b) Transverse Section (5003 Magnification Before Section and (b) Transverse Section (5003 Magnification Before
Reproduction) Reproduction)

TEST METHOD B—CHARPY IMPACT TEST FOR

Method A. Test Method B is applicable to S31803 and S32205. CLASSIFICATION OF STRUCTURES OF
A Possibly Affected Structure is likely to be associated with a DUPLEX STAINLESS STEELS
loss of Charpy impact toughness ranging from slight to severe.
8. Scope
An Affected Structure is associated with a severe loss of
Charpy impact toughness. A Centerline Structure may or may 8.1 This test method describes the procedure for conducting
not be detected by a Charpy test, depending on the orientation the Charpy impact test as a method of detecting the precipita-
tion of detrimental intermetallic phases in duplex stainless
of the Charpy specimen.
steels. The presence or absence of an indication of intermetallic
7.3 Test Method C—The ferric chloride corrosion test is a phase in this test is not necessarily a measure of performance
24-h test in 10 % ferric chloride. It will detect a loss of of the material in service with regard to any property other than
corrosion resistance associated with local depletion of chro- that measured directly. The Charpy procedure as here applied
mium and molybdenum as a result of the precipitation of is different from that as commonly applied for the determina-
chromium-rich and possibly molybdenum-rich phases, not tion of toughness and should not be used when characterization
limited to intermetallic phases. An Affected Structure is asso- of material toughness is the purpose of the testing.
ciated with significant weight loss in the corrosion test. A 8.2 The Charpy impact test may be used to evaluate mill
Possibly Affected Structure is likely to be associated with products, provided that it is possible to obtain a specimen of
significant weight loss in the corrosion test. relevant location and geometry.

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A 923

FIG. 4 S31803: Longitudinal Section (5003 Magnification Before

Reproduction)

TABLE 2 Applicability and Acceptance Criteria for

Test Method B

Grade Condition Acceptable Minimum Impact

Energy at −40°F (−40°C)A
S31803, S32205 base metal 40 ft-lb (54 J)
heat-affected zone 40 ft-lb (54 J)
weld metal 25 ft-lb (34 J)
B
S32750 base metal
A
Energy for a full-size specimen. Required energy for a subsize specimen is
reduced in direct proportion to the reduced area of the subsize specimen relative
to that of the full-size specimen.
B
The acceptable minimum impact energy shall be agreed upon by seller and
purchaser.

10. Apparatus
FIG. 3 Affected Structure in 8a S31803: (a) Longitudinal Section 10.1 The test apparatus shall be as described in Test
and (b) Transverse Section (5003 Magnification Before
Methods and Definitions A 370.
Reproduction)
11. Preparation of Test Specimens
8.3 Table 2 indicates the applicability and acceptance crite-
11.1 The test specimen shall be as described in Test Meth-
ria for Test Method B.
ods and Definitions A 370.
9. Rapid Screening Test 11.2 An impact test for the purpose of detecting intermetal-
lic phases shall consist of a single specimen taken from the
9.1 Before testing by the Charpy impact test, specimens of
product piece or lot to be represented.
the steel may be given a rapid screening test in accordance with
11.3 The test specimen may be aligned in either the longi-
the procedures of Test Method A, Sodium Hydroxide Etch Test
tudinal or transverse direction (see Note 3).
for Classification of Etch Structures of Duplex Stainless Steels.
Preparation, etching, and the classification of etch structures NOTE 3—The impact toughness of a transverse specimen from mill
are described therein. Specimens having an etch structure products of duplex stainless steels is typically one half to two thirds of that
described as Unaffected Structure in Test Method A will be of a longitudinal specimen.
essentially free of detrimental effect on impact toughness 11.4 Subsize specimens may be used for products with
related to the formation of intermetallic phase. Other mecha- thickness less than that of a full-size Charpy specimen. Subsize
nisms for loss of toughness may occur independently but are specimens should be as large as permitted by the product, in
beyond the scope of this test method. Specimens showing quarter-size increments.
Unaffected Structure in Test Method A are acceptable with 11.5 When this test is applied to a welded structure, or to
respect to the absence of intermetallic phases, without the any product having a less than uniform structure, particular
necessity of performing the Charpy test as described in Test attention should be paid to the location of the V-notch. For
Method B. All specimens having other than Unaffected Struc- example, in the heat-affected zone of a weld, the degree of
ture shall be tested by the Charpy impact test. intermetallic formation may vary significantly over short

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A 923
distances as a function of the local thermal cycle. In such cases, accordance with the procedures of Test Method A, Sodium
the placement of the V-notch may affect the measured result Hydroxide Etch Test for Classification of Etch Structures of
significantly. Duplex Stainless Steels. Preparation, etching, and the classifi-
cation of etch structures are described therein. Specimens
12. Procedure having an etch structure described as Unaffected Structure in
12.1 Perform the test in accordance with the procedures Test Method A will be essentially free of detrimental effects on
described in Test Methods and Definitions A 370. pitting corrosion resistance as related to the formation of an
12.2 Unless otherwise specified, perform the test at −40°F intermetallic phase. Other mechanisms for loss of pitting
(−40°C). resistance may occur independently but are beyond the scope
of this test method. Specimens showing Unaffected3 Structure
13. Acceptance Values and Retests in Test Method A are acceptable with respect to the absence of
13.1 Unless otherwise specified, the acceptance criteria intermetallic phases and need not be tested by the ferric
shall be as given in Table 2. chloride corrosion test as described in Test Method C. All
13.2 If a test specimen shows a value below the specified specimens having other than Unaffected Structure shall be
minimum, one retest of two specimens is permitted. For tested by the ferric chloride corrosion test.
acceptance, both retest specimens shall show a value at or
above the specified minimum value. 16. Apparatus
13.3 A product that has failed the Charpy impact test may, 16.1 Glass Beakers, 1000-mL, tall-form, or Erlenmeyer
at the option of the producer, be given a full anneal and flasks, 1000-mL, wide neck, or 50-mm (2-in.) diameter test
retested. tubes, or other suitable glass containers.
16.2 Glass Cradles (Fig. 5)—The dimensions of the cradle
TEST METHOD C—FERRIC CHLORIDE shall be restricted to those that will permit its passage through
CORROSION TEST FOR CLASSIFICATION OF the test container opening, a diameter of approximately 40 mm
STRUCTURES OF DUPLEX (1.6 in.) in the case of the Erlenmeyer flask.
STAINLESS STEELS 16.3 Water or Oil Bath, constant temperature.
14. Scope 17. Ferric Chloride Test Solution
14.1 This test method describes the procedure for conduct- 17.1 The test solution is prepared by dissolving 100 g of
ing the ferric chloride corrosion test for detecting the presence reagent-grade ferric chloride, FeCl3·6H2O, in 900 mL of
of detrimental intermetallic phases in duplex stainless steels. distilled water (approximately 6 % FeCl3 by weight). The
The presence or absence of corrosion attack in this test is not solution is filtered through glass wool or filter paper to remove
necessarily a measure of the performance of the material in insoluble particles.
other corrosive environments; in particular, it does not provide 17.2 The pH of the test solution shall be adjusted to
a basis for predicting resistance to forms of corrosion not approximately 1.3 prior to beginning the test by the addition of
associated with the precipitation of intermetallic phases (see HCl or NaOH, as required.
Note 4).
14.2 The ferric chloride corrosion test may be used to 18. Test Specimen
evaluate mill products, provided that it is possible to obtain a 18.1 Various shapes and sizes of test specimens may be
specimen of relevant location and geometry. used. For flat products, a specimen should be approximately 25
14.3 Table 3 indicates the applicability and acceptance by 50 mm (1 by 2 in.) by thickness. The full thickness of the
criteria for Test Method C. product should be included. In the case of heavier sections, the
specimen may be taken in a perpendicular orientation with
NOTE 4—Although this test method uses some equipment and proce-
dures similar to those of Test Method G 48, this test method should not be dimensions of approximately 6 by 25 mm (1⁄4 by 1 in.) by
confused with Test Method G 48. This test method does not determine the thickness. In very heavy sections, the thickness dimension of
critical pitting temperature or test for the suitability for use in a particular the specimen may be cut so that one half to two thirds of the
environment. This test method is designed solely for detection of the product thickness is tested.
precipitation of detrimental intermetallic phases in duplex stainless steels. 18.2 Other product forms may be cut for test specimens
convenient for testing, provided that the specimen exposes
15. Rapid Screening Test
surfaces representative of the full thickness of the product.
15.1 Before testing by the ferric chloride corrosion test, 18.3 After the specimens are cut, any material that may have
specimens of the steel may be given a rapid screening test in been affected by high temperature or deformation associated
with the cutting should be removed by machining or grinding
TABLE 3 Applicability and Acceptance Criteria for prior to testing.
Test Method C 18.4 For mill products, all surfaces of the specimen should
Grade Condition Test Maximum Acceptable be polished to a uniform finish at least equal to a 120-grit
Temperature Corrosion Rate Calculated
from Weight Loss
finish, or finer. Wet polishing is preferred. If used, dry
polishing should be performed slowly to prevent overheating.
S31803, S32205 base metal 25°C (77°F) 10 mdd
weld metal 22°C (72°F) 10 mdd Sharp edges of the specimen should be rounded, with care
taken to remove all burrs.

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A 923

FIG. 5 Examples of Glass Cradles That Can Be Used to Support

the Specimen

18.5 The surface of the specimen shall not be chemically 19.6 At the end of the 24-h test period, remove the specimen
passivated by treatments such as nitric, citric, or phosphoric from the solution, rinse with water, scrub with a soft bristle
acid, or pickled by treatments such as nitric hydrofluoric acid, brush under running water to remove corrosion products,
subsequent to grinding the surface. dipped in acetone or alcohol, and dried in air. Ultrasonic
18.6 For other than mill products, testing of a specimen with cleaning is a permitted alternative when there are corrosion
the surface in the as-fabricated condition may be relevant to the products that are difficult to remove.
application. 19.7 Weigh the specimen to 0.001 g or better and reserve for
18.7 The dimensions of the specimen are measured, and the examination.
total exposed surface area is calculated.
18.8 The specimen should be cleaned with magnesiumoxide 20. Acceptance Values
paste or equivalent, rinsed well with water, dipped in alcohol or 20.1 The corrosion rate is calculated in accordance with the
acetone, and air dried. The specimen shall be weighed to the weight loss and total surface area (see Note 5). Unless
nearest 0.001 g or better. It should be stored in a desiccator otherwise specified, the calculated corrosion rate shall not
until ready for testing. exceed 10 mdd (see Note 6).
19. Procedure NOTE 5—The corrosion rate is calculated in accordance with the
following: corrosion rate (mdd)
19.1 Perform the test using ferric-chloride solution with a = weight loss (mg)/[specimen area (dm2) 3 time (days)]
volume at least the larger of 150 mL or 20 mL/cm2(125 NOTE 6—It is probable that corrosion will occur by pitting when it does
mL/in.2) of the specimen surface area. Fill the test container occur. The calculation of a uniform corrosion rate would be an inappro-
with the required volume, transfer to the constant temperature priate method of expressing the pitting corrosion. However, in this case,
bath, and allow to come to equilibrium at the desired test the calculation of a corrosion rate is used primarily to normalize the
temperature. weight loss for the variety of specimen sizes and shapes permitted.
19.2 Unless otherwise specified, the test temperature for 20.2 If the specimen shows a corrosion rate in excess of 10
wrought products of S31803 and S32205 shall be 25°C (77°F), mdd, one retest on two new specimens from the same product
maintained within an accuracy of 61°C (2°F) during the test. is permitted. No retest specimen shall exhibit a corrosion rate
19.3 Unless otherwise specified, the test temperature for in excess of 10 mdd.
S31803 and S32205 products containing weldments shall be 20.3 At the option of the producer, a product that has failed
22°C (72°F), maintained within an accuracy of 61°C (2°F) the ferric-chloride corrosion test may be given a full anneal and
during the test. retested.
19.4 Unless otherwise specified, the test temperature for
S32750 products shall be 40°C (104°F), maintained within an 21. Precision and Bias
accuracy of 61°C (2°F) during the test. 21.1 No statement is made concerning either the precision
19.5 Place the specimen in the glass cradle and immerse in or bias of Test Methods A, B, or C for detecting the presence
the test solution once the temperature has been established. or absence of detrimental intermetallic phases in wrought
Maintain the test temperature throughout the test. Cover the duplex stainless steels because the results state merely whether
test container with a watchglass during the test period. Unless there is conformance to the criteria for success specified in the
otherwise specified, the test period shall be 24 h. procedure.

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A 923

APPENDIX

(Nonmandatory Information)

X1. EXAMPLE OF THE EFFECT OF THERMAL EXPOSURE ON TOUGHNESS AND

CORROSION RESISTANCE OF S31803

TABLE X1.1 Effect of Thermal ExposureA

Composition of Test Material

C Mn P S Si Cr Ni Mo N
0.023 1.44 0.022 0.001 0.49 22.3 5.60 3.13 0.182
Heat Treatment Condition CVN Impact Energy (ft-lb at −40°F (J at −40°C))B Critical Pitting Temperature (°C)C
Longitudinal Transverse
Mill annealed 185 (251) 127 (172) 35
1950°F (1066°C) + WQ 196 (266) 123 (167) not tested
1950°F (1066°C) + WQ + 5 min, 1550°F 42 (60) 25 (34) 20
1950°F (1066°C) + WQ + 10 min, 32 (43) 16 (22) 15
1550°F
1950°F (1066°C) + WQ + 15 min, 26 (35) 12 (16) not tested
1550°F
1950°F (1066°C) + WQ + 20 min, 21 (28) 9 (12) 15
1550°F
1950°F (1066°C) + air cool 198 (268) 133 (180) not tested
1950°F (1066°C) + slow cool 80 (108) 88 (119) 30
A
Davison, R. M., and Redmond, J. D., Paper No. 302, NACE Corrosion 91, 1991.
B 3
⁄8-in.(9.5-mm) plate, three-quarter size Charpy specimen.
C
CPT per Test Method G 48, Test Method A.

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