Designation: E 768 – 99

AMERICAN SOCIETY FOR TESTING AND MATERIALS

100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM

Standard Guide for

Preparing and Evaluating Specimens for Automatic
Inclusion Assessment of Steel1
This standard is issued under the fixed designation E 768; 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 4. Significance and Use

1.1 This guide2 covers two preparation methods for steel 4.1 Inclusion ratings done either manually using Test Meth-
metallographic specimens that will be analyzed for nonmetallic ods E 45 or automatically using Practice E 1122 or E 1245 are
inclusions with automatic image analysis (AIA) equipment. influenced by the quality of specimen preparation. This guide
The two methods of preparation are offered as accepted provides examples of proven specimen preparation methods
methods used to retain nonmetallic inclusions in steel. This that retain inclusions in polished steel specimens.
guide does not limit the user to these methods. 4.2 This guide provides a procedure to determine if the
1.2 A procedure to test the suitability of the prepared prepared specimens are of suitable quality for subsequent
specimen for AIA inclusion work, using differential interfer- rating of inclusions. None of these methods should be con-
ence contrast (DIC), is presented. strued as defining or establishing specific procedures or limits
of acceptability for any steel grade.
2. Referenced Documents
2.1 ASTM Standards: 5. Preparation Methods
E 3 Methods of Preparation of Metallographic Specimens3 5.1 Background:
E 7 Terminology Relating to Metallography3 5.1.1 The inclusions in the plane of polish must be fully
E 45 Test Methods for Determining the Inclusion Content preserved and clearly visible. Preparation should not produce
of Steel3 excessive relief around the perimeter of the inclusions that
E 883 Guide for Reflected-Light Photomicrography3 would exaggerate the size and number of inclusions on the
E 1122 Practice for Obtaining JK Inclusion Ratings Using plane of polish. In many cases, the preparation of specimens
Automatic Image Analysis3 for inclusion rating is more readily performed after the
E 1245 Practice for Determining the Inclusion or Second- specimens have been hardened by a suitable heat treatment
Phase Constituent Content of Metals by Automatic Image procedure (austenize, quench to fully martensitic structure,
Analysis3 temper at a relatively low temperature).
5.1.2 Cleanliness is an important consideration in all stages
3. Terminology of specimen preparation.
3.1 Definitions: 5.1.2.1 Heat-treated specimens should be wire brushed or
3.1.1 For definitions used in this practice, refer to Termi- shot blasted or have the surface ground to remove adherent
nology E 7. scale.
3.1.2 differential interference contrast microscopy—a com- 5.1.2.2 After completing the grinding steps and before
prehensive definition appears in Guide E 883, paragraph 11.8. performing the polishing steps, the specimens and specimen
3.2 Definitions of Terms Specific to This Standard: holders must be cleaned to prevent contamination of the next
3.2.1 rigid grinding disk—a non-fabric support surface, preparation step. Cleaning the specimens and specimen holders
such as a composite of metal/ceramic or metal/polymer, between each grinding step can eliminate contamination of
charged with an abrasive (usually 6 to 15-µm diamond par- coarse abrasives to the following finer preparation step.
ticles), and used as the fine grinding operation in a metallo- 5.1.2.3 After the preparation is complete, swab the surface
graphic preparation procedure. carefully with cotton and a water/soap solution containing a
corrosion inhibitor such as a machine coolant or ethyl alcohol
1
solution to remove any films or other debris that would
This test method is under the jurisdiction of ASTM Committee E-4 on interfere with the inclusion rating.
Metallography and is the direct responsibility of Subcommittee E04.01 on Sampling
Specimen Preparation, and Photography. 5.1.2.4 It is advisable to perform the inclusion analysis as
Current edition approved April 10, 1999. Published July 1999. soon as possible after preparation to minimize staining or other
2
Supporting data available from ASTM Headquarters. Request E04.1002. problems that can affect the analysis.
3
Annual Book of ASTM Standards, Vol 03.01.

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5.1.3 The two methods that follow have been found to be of steel grades. The relatively low pressures suggested in this
reliable procedures for retaining inclusions in steel and achiev- procedure will not necessarily result in a satisfactory polish for
ing the desired results when evaluated by DIC. There are other etching and the further evaluation of the specimen’s general
methods that will result in a quality specimen as revealed by microstructure. The pressures used in the following rigid disk
DIC. Each laboratory should develop preparation procedures procedure are more likely to result in a surface more satisfac-
for their materials so that the prepared surfaces meet the tory for revealing general microstructures.
requirements presented in 6 of this guide. 5.2.3 Grind the specimens on ANSI 80 grit (P80 FEPA)
5.1.4 As described in Methods E 3, the specimens may be silicon carbide paper to ensure all sectioning artifacts and
sectioned and mounted to ease handling during preparation. It deformation damage have been removed and the entire speci-
is advisable to use a mounting medium that is hard enough to men surface is co-planar to the grinding surface.
preserve edges and maintain flatness.
NOTE 2—If the sectioning method resulted in a smooth face and little
5.1.5 Abrasive grit size designations in this guide are deformation damage, and if after securing the specimens in a fixture for
expressed in the American National Standards Institute (ANSI) polishing, the entire surface of interest is co-planar to the grinding surface,
or Coated Abrasives Manufacturers Institute (CAMI) system then finer grit papers, such as ANSI 180 to 240 (P180 to P240 FEPA) can
units with the corresponding Federation of European Abrasive be used for the initial grinding step.
Procedure (FEPA) numbers in parentheses. Table 1 provides a 5.2.3.1 An adequate flow of water should remove all loos-
correlation between these two systems and the approximate ened abrasive and grinding debris from the paper during the
median particle diameter for a given grit size in micrometres. grinding procedure. The flow of water should ensure the
5.1.6 Most preparation systems apply pressure on the speci- specimen is kept cool during grinding.
mens being processed. The best pressure to be used for each 5.2.4 Continue grinding through the sequence of silicon
preparation step should be determined experimentally. Conver- carbide papers listed in Table 2. It may be necessary to clean
sions between applied force and pressure are discussed in the the samples between every grinding step to prevent contami-
Appendix X1. nation of the next preparation step.
NOTE 1—Care must be taken to protect the polished specimen surface 5.2.5 After completing the entire grinding operation, clean
from scratches or contaminants when using a specimen leveling device. the specimens thoroughly, using ethyl alcohol and cotton, then
5.2 Silicon Carbide Procedure: rinse and dry. Ultrasonic cleaning can be used.
5.2.1 A summary of the silicon carbide procedure can be 5.2.5.1 The use of a soap and water solution in an ultrasonic
found in Table 2. cleaner can attack non-metallic inclusions in some carbon and
5.2.2 When using a semi-automatic polishing equipment, low alloy steels, leading to an exaggeration in the inclusion’s
grinding and polishing should be performed using approxi- apparent size. Adding an inhibitor (such as that used as a
mately 18 kPa pressure per specimen. (For a specimen holder machining coolant) may reduce this size exaggeration.
containing six 32-mm mounts, a force of approximately 87 N 5.2.6 Polish the specimens using 3-µm diamond abrasive on
must be applied (see X1.4.2). a low nap cloth, such as woven wool, for 50 s. Clean and dry
5.2.2.1 Low pressures are recommended to ensure the the specimens as described in 5.2.5.
retention of an assortment of inclusion types found in a variety 5.2.7 Polish the specimens using a 1-µm diamond abrasive
on a high nap cloth for 50 s. Clean and dry the specimens as
TABLE 1 Comparison of ANSI (CAMI) versus FEPA versus described in 5.2.5.
Median Diameter of Grit Size in Micrometers 5.2.8 A final manual polishing step may be added, using
ANSIA (CAMI)B FEPAC Approximate Median 0.25-µm diamond abrasive on a low nap cloth for 10 to 20 s,
Diameter using relatively high pressure. Clean and dry the specimens as
(µm) described in 5.2.5.
60 P60 250 5.2.8.1 Ultrasonic cleaning is not recommended after the
80 P80 180
100 P100 150
final manual or automatic polishing step. Ultrasonic cleaning
120 P120 125 can cause cavitation damage, ultimately distorting the inclu-
150 P150 90 sion sizes.
180 P180 75
220 P220 63 NOTE 3—Depending on the material, it may be advisable to avoid water
240 P240 58.5 after polishing.
P280 52.2
280 P320 46.2 5.3 Rigid Grinding Disk Procedure:
320 P360 40.5 5.3.1 A summary of the rigid grinding disk procedure can be
P400 35.0
360 P500 30.2 found in Table 3.
400 P600 25.8 5.3.2 Semi-automatic grinding equipment is required, with
P800 21.8
specimens contained in a circular fixture for the entire proce-
500 P1000 18.3
600 P1200 15.3 dure. For 5.3.2-5.3.5, a pressure of 42 kPa should be applied
800 P2400 8.4 per specimen. (For a specimen holder containing six 32-mm
1200 P4000D 3.0
circular mounts, a force of approximately 203 N must be
A
ANSI - American National Standards Institute applied (see X1.4.3).
B
CAMI - Coated Abrasives Manufacturers Institute
C
FEPA - Federation of European Abrasive Producers 5.3.3 Grind for at least 15 s after achieving a co-planar
D
Not a FEPA designation condition, using a 150-grit alumina grinding stone at 1450 rpm

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TABLE 2 Preparation Method I Silicon Carbide Abrasive Paper Grinding
Surface Coolent/ Abrasive Size/Type Time ForceC Surface Relative Rotation
Lubricant ANSIA [FEPA]B (seconds) newtons [lbs] Speed
RPM
Planar Grinding
Paper Water 80 [P80] grit SIC 60 14 [2] 300 ComplementaryD
Fine Grinding
Paper Water 120 [P120] grit SIC 14 [2] 300 Complementary
Paper Water 240 [P240] grit SIC 60 14 [2] 300 Complementary
Paper Water 320 [P500] grit SIC 60 14 [2] 300 Complimentary
Paper Water 400 [P600] grit SIC 60 14 [2] 300 Complementary
Paper Water 600 [P1200] grit SIC 60 14 [2] 300 Complimentary
Paper Water 800[P2400] grit SIC 60 14 [2] 300 Complementary
Rough Polishing
NAP free cloth Extending fluid 3 µm diamond 50 14 [2] 150 Complementary
Final Polishing
Low nap cloth Extending fluid 1 µm diamond 50 14 [2] 150 Complementary
Optional Polishing (manual)
Low nap cloth Extending fluid 1 µm diamond 50 relatively high NA NAE
A
American National Standards Institute (ANSI) designation of grit size.
B
Federation of European Producers of Abrasives (FEPA) designation of grit size.
C
Force per 3-mm (1.25-in.) diameter specimen.
D
Complementary rotation, surface and specimens spin in same direction.
E
Since this optional step is completed manually, these two categories are not applicable.

TABLE 3 Preparation Method II - Rigid Grinding Disk Procedure

Surface Coolant/ Abrasive Size/Type ANSIA Time - seconds ForceC Surface Speed Relative Rotation
Lubricant [FEPA]B newtons [lbs] RPM
Planar Grinding
Alumina/zirconia paper Water 80 [P80] grit >15 34 [8] 300 ComplementaryD
Or
Alumina grinding stone Water 150 [P150] grit >15 34 [8] 1450 Complementary
Fine Grinding
Rigid grinding disk Alcohol/glycol 9 µm diamond 180 34 [8] 150 Complementary
Rough Polishing
Napless or stiff napped cloth Alcohol/glycol 3 µm diamond 240 34 [8] 150 Complementary
Final Polishing
Soft short napped cloth Alcohol/glycol 1 µm diamond 120 34 [8] 150 Complementary
Optional Polishing
Porous Synthetic Cloth Water Alkaline Colloidal Silica or 90 100 [23] 150 Complementary
Acidic Colloidal AluminaE
A
American National Standards Institute (ANSI) designation of grit size.
B
Federation of European Producers of Abrasives (FEPA) designation of grit size.
C
Force per 32-mm (1.25-in.) diameter specimen.
D
Complementary rotation surface, and specimens spin in same direction.
E
Water is substituted for the colloidal oxide during the last 20 s.

or 80-grit (P80 FEPA) alumina/zirconia grinding paper at 300 machining coolant) may reduce this size exaggeration.
rpm. 5.3.5 Rough polish using 3-µm diamond on a napless cloth
5.3.3.1 An adequate flow of water should remove all loos- (silk or non-woven chemotextile) or a low nap cloth (woven
ened abrasive and grinding debris from the paper during the wool) for 4 min at 150 rpm using alcohol/glycol lubricant.
grinding procedure. The flow of water should ensure the Clean as in 5.3.4.
specimen is kept cool during grinding. 5.3.6 Final polish using 1-µm diamond on a high nap cloth
5.3.3.2 It may be necessary to clean the samples between for 2 min at 150 rpm, using alcohol/glycol lubricant. Clean as
every grinding step to prevent contamination of the next in 5.3.4.
preparation step. 5.3.6.1 Ultrasonic cleaning is not recommended after the
5.3.4 Finish grind using 9-µm diamond on a rigid grinding final polishing step. Ultrasonic cleaning can cause cavitation
disk for 3 m at 150 rpm, using an alcohol/glycol lubricant. damage, ultimately distorting the inclusion sizes.
Clean the specimens and fixture thoroughly (ultrasonic clean- 5.3.7 An optional oxide-polishing step, using a porous
ing is helpful) with alcohol and cotton, then dry with forced air. synthetic cloth with either alkaline colloidal silica or acidic
5.3.4.1 The use of a soap and water solution in an ultrasonic colloidal alumina, may be used if necessary to eliminate fine
cleaner can attack non-metallic inclusions in some carbon and scratches. The conditions are 90 s at 150 rpm, 100 N, with
low alloy steels, leading to an exaggeration in the inclusion’s water substituted for the colloidal oxide during the last 20 s.
apparent size. Adding an inhibitor (such as that used as a Clean as in 5.3.4.

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6. DIC Evaluation Method4 There could be a critical trough configuration beyond which
6.1 A microscope equipped with DIC illumination at mag- the bright troughs turn black at some point in the transition to
nifications of about 100x and 500x should be used while bright field illumination, and the inclusions appear to become
developing the preparation procedure to verify the true surface larger. This condition indicates insufficient preparation. (The
topography of properly prepared specimens. The sensitive tint use of a filar eyepiece may be helpful at this point to determine
condition, using a first order gypsum (1l) plate, is the most whether the inclusion through has widened)
useful mode of DIC illumination (plane areas magenta; inclu- 6.3.2 Narrow troughs can be accepted as harmless if they
sions dark). vanish into the background when the polarizer is opened a
6.2 Observation at 100x will reveal whether residual small part of its range.
scratches are present and whether background relief is evident. 6.4 Some fine scratches from final polishing will usually be
6.3 At 500x in the DIC sensitive tint condition, all of the seen under DIC at 500x. These normally also vanish on
edges of inclusion particles should be sharp and recognizable opening the polarizer and, therefore, should not affect quanti-
as sharp edges. Narrow bright lines indicating narrow ditches tative measurement at lower magnification.
at some inclusion edges may, however, still be seen. A test may NOTE 4—While highly instructive, the DIC examination remains sub-
be made to determine whether these ditches will be detected by jective with respect to the question of whether a reproducible and accurate
the image analysis system. surface preparation has been obtained. Tests by actual measurement are
6.3.1 The polarizer is slowly rotated away from the full DIC necessary to determine that errors in specimen preparation were not
position and the inclusion edges watched for apparent motion. contributory to outlier observations.

7. Keywords
4
A colored plate, consisting of six micrographs that illustrate the use of DIC in
determining a properly prepared sample (at 100x and 500x), is available from 7.1 automatic image analysis; differential interference con-
ASTM Headquarters. Order PCN 12-507680-22. trast; inclusions; specimen preparation; steel

APPENDIX

(Nonmandatory Information)

X1. APPLIED LOAD CONVERSIONS

X1.1 Automatic preparation machines commonly display X1.4.1 Example 1—What is the force in pound-force if 87
applied force in either pound-force (lbf) or newtons (N). The N is applied?
ability to convert from one unit to another may be necessary ~87 N! 3 ~0.225! 5 19.6 lbf (X1.1)
when trying to interpret a documented procedure.
X1.4.2 Example 2—What is the applied load, in newtons,
X1.1.1 To convert from pound-force to newton, multiply the required to apply a pressure of 18 kPa to an individual
pound-force value by 4.5. specimen in a holder containing six 32-mm circular mounts?
X1.1.2 To convert from newton to pound-force, multiply the
Pressure 5 (Force)/(Area), therefore . . . Force 5 (Pressure)
newton value by 0.225.
3 (Area)
X1.2 When multiple specimens are held in a holder, the Area 5 P r25 P (16)25 804.25 mm2
applied force must be divided by the number of specimens in Total Area 5 (6 mounts) 3 (804.25 mm2) 5 4825.5 mm2
the holder to determine the load per specimen. Some auto- 18 kPa 5 18 000 Pa 5 18 000 N/m25 0.018 N/mm2
mated machines apply the load individually to each specimen Therefore,
and display the applied load accordingly. Force 5 (0.018 N/mm2) 3 4825.5 mm2) 5 86.9 N
X1.4.3 Example 3—What is the applied load, in newtons,
X1.3 Caution should be taken when using automated required to apply a pressure of kPa to an individual specimen
machines that display pressure in pound-force per square inch in a holder containing six 32-mm mounts?
(psi). Typically, the machine is displaying the air pressure Pressure 5 (Force)/(Area), therefore . . . Force 5 (Pressure)
within the loading cylinder and not the true pressure applied to 3 (Area)
either the specimen holder or each individual specimen.
Area 5 P r25 P (16)25 804.25 mm2
X1.4 When converting from a force to a pressure, the Total Area 5 (6 mounts) 3 (804.25 mm25 4825.5 mm2
surface area of the specimen must be determined. The value of 42 kPa 5 42 000 Pa 5 42 000 N/m25 0.042 N/mm2
force is then divided by the contact area to determine the Therefore,
required pressure. Force 5 (0.042 N/mm2) 3 4825.5 mm2) 5 203 N

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