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Astm A923 23

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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: A923 − 23

Standard Test Methods for


Detecting Detrimental Intermetallic Phase in Duplex
Austenitic/Ferritic Stainless Steels1
This standard is issued under the fixed designation A923; 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* 1.6 The presence of detrimental intermetallic phases is


1.1 The purpose of these test methods is to allow detection readily detected in all three tests, provided that a sample of
of the presence of intermetallic phases in certain duplex appropriate location and orientation is selected. Because the
stainless steels as listed in Table 1, Table 2, and Table 3 to the occurrence of intermetallic phases is a function of temperature
extent that toughness or corrosion resistance is affected signifi- and cooling rate, it is essential that the tests be applied to the
cantly. These test methods will not necessarily detect losses of region of the material experiencing the conditions most likely
toughness or corrosion resistance attributable to other causes. to promote the formation of an intermetallic phase. In the case
Similar test methods for other duplex stainless steels are of common heat treatment, this region will be that which
described in Test Method A1084, but the procedures described cooled most slowly. Except for rapidly cooled material, it may
in this standard differ significantly from Test Methods A, B, be necessary to sample from a location determined to be the
and C in A1084. most slowly cooled for the material piece to be characterized.
1.7 The tests do not determine the precise nature of the
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1.2 Duplex (austenitic-ferritic) stainless steels are suscep-
tible to the formation of intermetallic compounds during detrimental phase but rather the presence or absence of an
exposures in the temperature range from approximately 600 to intermetallic phase to the extent that it is detrimental to the

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1750 °F (320 to 955 °C). The speed of these precipitation toughness and corrosion resistance of the material.
1.8 Examples of the correlation of thermal exposures, the
reactions is a function of composition and thermal or thermo-

tance.
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occurrence of intermetallic phases, and the degradation of
mechanical history of each individual piece. The presence of
toughness and corrosion resistance are given in Appendix X1
these phases is detrimental to toughness and corrosion resis-
and Appendix X2.
1.3 Correct heat treatment of duplex stainless steels can 1.9 The values stated in either inch-pound or SI units are to
ASTM A923-23
eliminate these detrimental phases. Rapid cooling of the be regarded as the standard. The values given in parentheses
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product provides the maximum resistance to formation of are for information only.
detrimental phases by subsequent thermal exposures. 1.10 This standard does not purport to address all of the
1.4 Compliance with the chemical and mechanical require- safety concerns, if any, associated with its use. It is the
ments for the applicable product specification does not neces- responsibility of the user of this standard to establish appro-
sarily indicate the absence of detrimental phases in the product. priate safety, health, and environmental practices and deter-
1.5 These test methods include the following: mine the applicability of regulatory limitations prior to use.
1.5.1 Test Method A—Sodium Hydroxide Etch Test for 1.11 This international standard was developed in accor-
Classification of Etch Structures of Duplex Stainless Steels dance with internationally recognized principles on standard-
(Sections 3 – 7). ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
1.5.2 Test Method B—Charpy Impact Test for Classification
mendations issued by the World Trade Organization Technical
of Structures of Duplex Stainless Steels (Sections 8 – 13).
Barriers to Trade (TBT) Committee.
1.5.3 Test Method C—Ferric Chloride Corrosion Test for
Classification of Structures of Duplex Stainless Steels (Sec-
2. Referenced Documents
tions 14 – 20).
2.1 ASTM Standards:2
1
These test methods are under the jurisdiction of ASTM Committee A01 on
Steel, Stainless Steel and Related Alloysand are the direct responsibility of
2
Subcommittee A01.14 on Methods of Corrosion Testing. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 15, 2023. Published June 2023. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1994. Last previous edition approved in 2022 as A923 – 22. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/A0923-23. 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

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A923 − 23
A370 Test Methods and Definitions for Mechanical Testing 4.3 Variable Resistance (see Note 1).
of Steel Products 4.4 Cathode—A cylindrical piece of conductive metal.
A1084 Test Method for Detecting Detrimental Phases in
Lean Duplex Austenitic/Ferritic Stainless Steels 4.5 Large Electric Clamp, to hold the specimen to be
G48 Test Methods for Pitting and Crevice Corrosion Resis- etched.
tance of Stainless Steels and Related Alloys by Use of 4.6 Metallurgical Microscope, for examination of etched
Ferric Chloride Solution microstructures to 400 to 500 diameters.
TEST METHOD A—SODIUM HYDROXIDE ETCH 4.7 Electrodes of the Etching Cell—The specimen to be
TEST FOR CLASSIFICATION OF ETCH etched is made the anode, and a cylindrical piece of metal as
STRUCTURES OF DUPLEX STAINLESS STEELS large as the specimen to be etched is made the cathode.
4.8 Electrolyte, sodium hydroxide (NaOH), reagent grade.
3. Scope
NOTE 1—The variable resistance and ammeter are placed in the circuit
3.1 The sodium hydroxide etch test may be used for the to measure and control the current on the specimen to be etched.
acceptance of material but not for rejection. This test method
may be used with other evaluation tests to provide a rapid 5. Preparation of Test Specimens
method for identifying those specimens that are free of
detrimental intermetallic phases as measured in these other 5.1 For mill products, examination shall be made on a
tests. longitudinal or transverse section. For cast products, examina-
tion shall be made on a separately cast test coupon which was
3.2 The sodium hydroxide etch test may be used to screen heat treated in the same furnace load as the casting it
specimens intended for testing in Test Method B, Charpy represents. Unless otherwise specified, selection of the test
Impact Test for Classification of Structures of Duplex Stainless coupon size shall be at the discretion of the producer. Because
Steels, and in Test Method C, Ferric Chloride Corrosion Test high temperature or mechanical deformation associated with
for Classification of Structures of Duplex Stainless Steels. particular cutting processes may alter the structure of the steel,

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3.3 Reference photomicrographs are provided to show clas- the cutting of the test specimen should be by a technique that
sifications of etch structures of a particular stainless steel type prevents these effects. Alternatively, after the specimens are
that are equivalent to acceptable or to possibly unacceptable cut, any material that may have been affected by high tempera-
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performance for each practice. When Test Method A is used as
a screening test for Test Method B or Test Method C,
ture or deformation associated with the cutting should be
removed by machining or wet grinding prior to testing.

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specimens having acceptable etch structures need not be
subjected to Test Method B or Test Method C.
5.2 For mill products, the specimen should allow for a
survey across the full thickness of the section or, in the case of
3.4 Table 1 indicates the applicability and acceptance crite- a heavy section, a survey from one surface through the
ria for Test Method A. When Test Method A is specified as an mid-thickness of the section. The specimen shall include the
ASTM A923-23
acceptance test, specimens having other than acceptable etch mid-thickness.
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structures may, at the option of the producer, be tested by Test 5.3 For cast materials, the specimen shall be taken at
Method B or Test Method C. approximately 1/4T.
3.5 The steel shall be tested in the final solution heat treated 5.4 Polishing—On all materials, cross-sectional surfaces
condition or such other conditions as are agreed upon between should be polished to a metallographic finish suitable for
the producer and the user. examination at 400× after etching. Specimens containing welds
4. Apparatus should include base metal, weld heat–affected zone, and weld
metal. The area to be etched may be prepared by grinding to an
4.1 Source of Direct Current—Battery, generator, or rectifier 80- or 120-grit finish on a grinding belt or wheel without
capable of supplying approximately 15 V and 20 A. excessive heating and then by polishing on successively finer
4.2 Ammeter—Range from 0 to 30 A (see Note 1). emery papers, No. 1, 1⁄2, 1⁄0, 2⁄0, 3⁄0, and finer. Other methods of
polishing may be acceptable.

TABLE 1 Applicability and Acceptance Criteria for


5.5 Etching Solution—The solution for etching is prepared
Test Method A by adding 40 g of reagent grade sodium hydroxide (NaOH) to
Acceptable Nonacceptable
100 g of distilled water.
Grade
Etch Structure Etch Structure 5.6 Etching Conditions—The polished specimen should be
S82441, S31803, unaffected possibly affected etched at approximately 1 to 3 V dc, for 5 to 60 s (see Note 2).
S32205, S32750, structure (Fig. 1, structure (Fig. 3, Fig. 4)
S32760, Fig. 2) NOTE 2—When etching is performed at 1 to 3 V dc with a platinum
S32550,S32520,
cathode for 5 to 60 s, any intermetallic phase is revealed by yellow, then
J92205, J93404
affected structure (Fig. 5,
brown, staining, followed by staining of the ferrite.
Fig. 6) 5.7 Rinsing—Following etching, the specimen should be
centerline structure (Fig.
7) rinsed thoroughly in hot water and in acetone or alcohol,
followed by air drying.

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A923 − 23
6. Classification of Etch Structures
6.1 The etched surface shall be examined on a metallurgical
microscope at 400 to 500×.
6.2 The etched cross-sectional areas should be examined
thoroughly by complete traverse of the full sample and across
all zones such as weld metal, weld-affected zones, and base
metal on specimens containing welds.
6.3 The etch structures are classified into the following
types:
6.3.1 Unaffected Structure (Fig. 1, Fig. 2)—The ferrite has
been etched without revelation of intermetallic phase. The
interphase boundaries are smooth.
6.3.2 Possibly Affected Structure (Fig. 3, Fig. 4)—The
ferrite has been etched with isolated indications of possible
intermetallic phase. The interphase boundaries may show a fine
waviness.
6.3.3 Affected Structure (Fig. 5, Fig. 6)—The indications of
FIG. 2 (a) J92205: Unaffected Structure-Statically Cast (400× Mag-
an intermetallic phase are readily revealed before or simulta- nification)
neously with the staining of the ferrite during etching.

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ASTM A923-23
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FIG. 2 (b) J92205: Unaffected Structure-Centrifugally Cast (400×


Magnification) (continued)

6.3.4 Centerline Structure (Fig. 7)—An intermetallic phase


is observed as a continuous or semi-continuous phase in the
mid-thickness region of the product, with or without the
affected structure outside of the mid-thickness region, indica-
tive of segregation.

7. Interpretation and Use of the Etch Structure


Classifications
7.1 When Test Method A is used as a screening test, the use
of these etch structures depends on the test method for which
the specimens are being screened. Important characteristics of
each of the test methods are described as follows.
7.2 Test Method B—The Charpy impact test detects reduc-
tions in toughness from that of the optimal composition and
FIG. 1 Unaffected Structure in S31803: (a) Longitudinal Section
processing. Such reductions may be attributable to intermetal-
and (b) Transverse Section (500× Magnification Before Reproduc- lic phases or to other causes not necessarily detectable by Test
tion) Method A. A Possibly Affected Structure is likely to be

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A923 − 23

FIG. 4 (a) J92205: Possibly Affected Structure-Statically Cast


(400× Magnification)

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ASTM A923-23
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FIG. 3 Possibly Affected Structure in S31803: (a) Longitudinal
Section and (b) Transverse Section (500× Magnification Before
Reproduction)

associated with a loss of Charpy impact toughness ranging FIG. 4 (b) J92205: Possibly Affected Structure-Centrifugally Cast
from slight to severe. An Affected Structure is associated with (400× Magnification) (continued)
a severe loss of Charpy impact toughness. A Centerline
Structure may or may not be detected by a Charpy test, TEST METHOD B—CHARPY IMPACT TEST FOR
depending on the orientation of the Charpy specimen. CLASSIFICATION OF STRUCTURES OF
7.3 Test Method C—The ferric chloride corrosion test is a DUPLEX STAINLESS STEELS
24-h test in 10 % ferric chloride. It will detect a loss of
corrosion resistance associated with local depletion of chro- 8. Scope
mium and molybdenum as a result of the precipitation of 8.1 This test method describes the procedure for conducting
chromium-rich and possibly molybdenum-rich phases, not the Charpy impact test as a method of detecting the precipita-
limited to intermetallic phases. An Affected Structure is asso- tion of detrimental intermetallic phases in duplex stainless
ciated with significant weight loss in the corrosion test. A steels. The presence or absence of an indication of intermetallic
Possibly Affected Structure is likely to be associated with phase in this test is not necessarily a measure of performance
significant weight loss in the corrosion test. of the material in service with regard to any property other than

4
A923 − 23

FIG. 7 S31803: Longitudinal Section (500× Magnification Before


Reproduction)

that measured directly. The Charpy procedure as here applied


is different from that as commonly applied for the determina-
tion of toughness and should not be used when characterization
of material toughness is the purpose of the testing.
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8.2 The Charpy impact test may be used to evaluate mill and
cast products, provided that it is possible to obtain a specimen
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of relevant location and geometry.
8.3 Table 2 indicates the applicability and acceptance crite-
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ria for Test Method B.
9. Rapid Screening Test
9.1 Before testing by the Charpy impact test, specimens of
ASTM A923-23
the steel may be given a rapid screening test in accordance with
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FIG. 5 Affected Structure in 8a S31803: (a) Longitudinal Section the procedures of Test Method A, Sodium Hydroxide Etch Test
and (b) Transverse Section (500× Magnification Before Reproduc- for Classification of Etch Structures of Duplex Stainless Steels.
tion) Preparation, etching, and the classification of etch structures
are described therein. Specimens having an etch structure
described as Unaffected Structure in Test Method A will be
essentially free of detrimental effect on impact toughness

TABLE 2 Applicability and Acceptance Criteria for


Test Method B
Test Minimum Impact
Grade Condition
Temperature EnergyA
S82441 base metal –40 °F (–40 °C) 40 ft-lb (54 J)A
S31803, base metal –40 °F (–40 °C) 40 ft-lb (54 J)A
S32205,
J92205
heat-affected –40 °F (–40 °C) 40 ft-lb (54 J)A
zone
weld metal –40 °F (–40 °C) 25 ft-lb (34 J)A
B
S32750, base metal –40 °F (–40 °C)
S32760
J93404 base metal –50 °F (–46 °C) 40 ft-lb (54 J)A
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. Test may be conducted at a temperature below the
specified temperature.
B
FIG. 6 J92205: Affected Structure (400× Magnification) The acceptable minimum impact energy shall be agreed upon by seller and
purchaser.

5
A923 − 23
related to the formation of intermetallic phase. Other mecha- TEST METHOD C—FERRIC CHLORIDE
nisms for loss of toughness may occur independently but are CORROSION TEST FOR CLASSIFICATION OF
beyond the scope of this test method. Specimens showing STRUCTURES OF DUPLEX
Unaffected Structure in Test Method A are acceptable with STAINLESS STEELS
respect to the absence of intermetallic phases, without the
necessity of performing the Charpy test as described in Test 14. Scope
Method B. All specimens having other than Unaffected Struc- 14.1 This test method describes the procedure for conduct-
ture shall be tested by the Charpy impact test. ing the ferric chloride corrosion test for detecting the presence
of detrimental intermetallic phases in duplex stainless steels.
10. Apparatus The presence or absence of corrosion attack in this test is not
10.1 The test apparatus shall be as described in Test necessarily a measure of the performance of the material in
Methods and Definitions A370. other corrosive environments; in particular, it does not provide
a basis for predicting resistance to forms of corrosion not
11. Preparation of Test Specimens associated with the precipitation of intermetallic phases (see
11.1 The test specimen shall be as described in Test Meth- Note 4).
ods and Definitions A370. 14.2 The ferric chloride corrosion test may be used to
11.2 An impact test for the purpose of detecting intermetal- evaluate mill products, provided that it is possible to obtain a
lic phases shall consist of a single specimen taken from the specimen of relevant location and geometry.
product piece or lot to be represented. 14.3 Table 3 indicates the applicability and acceptance
11.3 For mill products, the test specimen may be aligned in criteria for Test Method C.
either the longitudinal or transverse direction (see Note 3). For NOTE 4—Although this test method uses some equipment and proce-
castings, the test specimen shall be parallel to the side of the dures similar to those of Test Methods G48, this test method should not be
test coupon; the notch may be either parallel to or perpendicu- confused with Test Methods G48. This test method does not determine the
lar to the coupon surface. critical pitting temperature or test for the suitability for use in a particular

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NOTE 3—The impact toughness of a transverse specimen from mill
products of duplex stainless steels is typically one half to two thirds of that
environment. This test method is designed solely for detection of the
precipitation of detrimental intermetallic phases in duplex stainless steels.

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of a longitudinal specimen. 15. Rapid Screening Test
11.4 Subsize specimens may be used for products with 15.1 Before testing by the ferric chloride corrosion test,

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thickness less than that of a full-size Charpy specimen. Subsize specimens of the steel may be given a rapid screening test in
specimens should be as large as permitted accordance with the procedures of Test Method A, Sodium
quarter-size increments. Hydroxide Etch Test for Classification of Etch Structures of
11.5 When this test is applied to a welded structure, or to Duplex Stainless Steels. Preparation, etching, and the classifi-
any product having a less than uniform structure,ASTM A923-23
particular cation of etch structures are described therein. Specimens
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attention should be paid to the location of the V-notch. For having an etch structure described as Unaffected Structure in
example, in the heat-affected zone of a weld, the degree of Test Method A will be essentially free of detrimental effects on
intermetallic formation may vary significantly over short pitting corrosion resistance as related to the formation of an
distances as a function of the local thermal cycle. In such cases, intermetallic phase. Other mechanisms for loss of pitting
the placement of the V-notch may affect the measured result resistance may occur independently but are beyond the scope
significantly. of this test method. Specimens showing Unaffected Structure
in Test Method A are acceptable with respect to the absence of
12. Procedure intermetallic phases and need not be tested by the ferric
12.1 Perform the test in accordance with the procedures chloride corrosion test as described in Test Method C. All
described in Test Methods and Definitions A370. specimens having other than Unaffected Structure shall be
tested by the ferric chloride corrosion test.
12.2 The test temperature shall be as specified in Table 2 for
the grade being evaluated.
TABLE 3 Applicability and Acceptance Criteria for
13. Acceptance Values and Retests
Test Method C
13.1 Unless otherwise specified, the acceptance criteria Maximum Acceptable
Test
shall be as given in Table 2. Grade Condition
Temperature
Corrosion Rate Calculated
from Weight Loss
13.2 If a test specimen shows a value below the specified S82441 base metal 15 °C (59 °F) 10 mdd
minimum, one retest of two specimens is permitted. For S31803, base metal 25 °C (77 °F) 10 mdd
acceptance, both retest specimens shall show a value at or S32205
weld metal 22 °C (72 °F) 10 mdd
above the specified minimum value. S32750 base metal 40 °C (104 °F) 10 mdd
13.3 A product that has failed the Charpy impact test may, S32760 base metal 40 °C (104 °F) 10 mdd
S32550 base metal 40 °C (104 °F) 10 mdd
at the option of the producer, be given a full anneal and S32520 base metal 40 °C (104 °F) 10 mdd
retested.

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A923 − 23
16. Apparatus 18.3 After the specimens are cut, any material that may have
16.1 Glass Beakers, 1000 mL, tall-form, or Erlenmeyer been affected by high temperature or deformation associated
flasks, 1000 mL, wide neck, or 50 mm (2-in.) diameter test with the cutting should be removed by machining or grinding
tubes, or other suitable glass containers. prior to testing.
16.2 Glass Cradles (Fig. 8)—The dimensions of the cradle 18.4 For mill products, all surfaces of the specimen should
shall be restricted to those that will permit its passage through be polished to a uniform finish at least equal to a 120-grit
the test container opening, a diameter of approximately 40 mm finish, or finer. Wet polishing is preferred. If used, dry
(1.6 in.) in the case of the Erlenmeyer flask. polishing should be performed slowly to prevent overheating.
Sharp edges of the specimen should be rounded, with care
16.3 Water or Oil Bath, constant temperature.
taken to remove all burrs.
17. Ferric Chloride Test Solution 18.5 The surface of the specimen shall not be chemically
17.1 The test solution is prepared by dissolving 100 g of passivated by treatments such as nitric, citric, or phosphoric
reagent-grade ferric chloride, FeCl3·6H2O, in 900 mL of acid, or pickled by treatments such as nitric hydrofluoric acid,
distilled water (approximately 6 % FeCl3 by weight). The subsequent to grinding the surface.
solution is filtered through glass wool or filter paper to remove 18.6 For other than mill products, testing of a specimen with
insoluble particles. the surface in the as-fabricated condition may be relevant to the
17.2 The pH of the test solution shall be adjusted to application.
approximately 1.3 prior to beginning the test by the addition of
18.7 The dimensions of the specimen are measured, and the
HCl or NaOH, as required.
total exposed surface area is calculated.
18. Test Specimen 18.8 The specimen should be cleaned with magnesiumoxide
18.1 Various shapes and sizes of test specimens may be paste or equivalent, rinsed well with water, dipped in alcohol or
used. For flat products, a specimen should be approximately acetone, and air dried. The specimen shall be weighed to the

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25 mm by 50 mm (1 in. by 2 in.) by thickness. The full
thickness of the product should be included. In the case of
nearest 0.001 g or better. It should be stored in a desiccator
until ready for testing.

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heavier sections, the specimen may be taken in a perpendicular
19. Procedure
orientation with dimensions of approximately 6 mm by 25 mm
(1⁄4 in. by 1 in.) by thickness. In very heavy sections, the
19.1 Perform the test using ferric-chloride solution with a
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thickness dimension of the specimen may be cut so that one
volume at least the larger of 150 mL or 20 mL/cm (125
half to two thirds of the product thickness is tested. 2
mL/in. ) of the specimen surface area. Fill the test container
2

18.2 Other product forms may be cut for test specimens with the required volume, transfer to the constant temperature
convenient for testing, provided that the specimen ASTM A923-23
exposes bath, and allow to come to equilibrium at the desired test
surfaces representative of the full thickness of the product. temperature.
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FIG. 8 Examples of Glass Cradles That Can Be Used to Support


the Specimen

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