ASTM E1351-01(2012)

Standard Practice for Production and Evaluation of Field Metallographic Replicas

SIGNIFICANCE AND USE
4.1 Replication is a nondestructive sampling procedure that records and preserves the topography of a metallographically prepared surface as a negative relief on a plastic film (replica). The replica permits the examination and analysis of the metallographically prepared surface on the LM or SEM.  
4.2 Enhancement procedures for improving replica contrast for microscopic examination are utilized and sometimes necessary (see 8.1).Note 1—It is recommended that the purchaser of a field replication service specify that each replicator demonstrate proficiency by providing field prepared replica metallography and direct LM and SEM comparison to laboratory prepared samples of an identical material by grade and service exposure.
SCOPE
1.1 This practice covers recognized methods for the preparation and evaluation of cellulose acetate or plastic film replicas which have been obtained from metallographically prepared surfaces. It is designed for the evaluation of replicas to ensure that all significant features of a metallographically prepared surface have been duplicated and preserved on the replica with sufficient detail to permit both LM and SEM examination with optimum resolution and sensitivity.  
1.2 This practice may be used as a controlling document in commercial situations.  
1.3 The values stated in SI units are to be regarded as the standard. Inch-pound units given in parentheses are for information only.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

• Status: Historical
• Publication Date: 30-Sep-2012
• ICS: 77.040.99 - Other methods of testing of metals
• Technical Committee: E04 - Metallography
• Drafting Committee: E04.01 - Specimen Preparation

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E1351 − 01 (Reapproved 2012)
Standard Practice for
Production and Evaluation of Field Metallographic Replicas
This standard is issued under the fixed designation E1351; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
INTRODUCTION
Replication is a nondestructive sampling procedure which records and preserves the topography of
a metallographic specimen as a negative relief on a plastic film. The microstructural replica can be
examined using a light microscope (LM) or scanning electron microscope (SEM) for subsequent
analysis. Specimens examined in the SEM are vacuum coated with vaporized carbon or a suitable
metal to provide contrast and conductivity. The convenience of the replication process makes it
suitable for obtaining microstructures from field locations for subsequent examination and analysis in
a laboratory. The proper preparation of the test surface and of the replica itself is of paramount
importance and must receive careful attention. Because of the diversity of metallographic equipment
available and the wide range of environments in which replication is conducted, the preparation of
replicas of high quality should be viewed as a skilled process for which there exists a variety of
techniques that achieve satisfactory results.
This practice presents some guidelines on the preparation of metallic surfaces and production of
replicas and guidelines on evaluation of replica quality. It does not attempt to limit the variations in
technique developed by skilled metallographers, each of which may produce acceptable replicas.
1. Scope 2. Referenced Documents
1.1 This practice covers recognized methods for the prepa- 2.1 ASTM Standards:
ration and evaluation of cellulose acetate or plastic film A335/A335MSpecification for Seamless Ferritic Alloy-
replicas which have been obtained from metallographically Steel Pipe for High-Temperature Service
prepared surfaces. It is designed for the evaluation of replicas E3Guide for Preparation of Metallographic Specimens
to ensure that all significant features of a metallographically E7Terminology Relating to Metallography
prepared surface have been duplicated and preserved on the E407Practice for Microetching Metals and Alloys
replica with sufficient detail to permit both LM and SEM
3. Terminology
examination with optimum resolution and sensitivity.
3.1 Definitions—For definitions of terms used in this
1.2 This practice may be used as a controlling document in
practice, refer to Terminology E7.
commercial situations.
1.3 The values stated in SI units are to be regarded as the
4. Significance and Use
standard. Inch-pound units given in parentheses are for infor-
4.1 Replication is a nondestructive sampling procedure that
mation only.
records and preserves the topography of a metallographically
1.4 This standard does not purport to address all of the
prepared surface as a negative relief on a plastic film (replica).
safety concerns, if any, associated with its use. It is the
The replica permits the examination and analysis of the
responsibility of the user of this standard to establish appro-
metallographically prepared surface on the LM or SEM.
priate safety and health practices and determine the applica-
4.2 Enhancement procedures for improving replica contrast
bility of regulatory limitations prior to use.
for microscopic examination are utilized and sometimes nec-
essary (see 8.1).
This practice is under the jurisdiction of ASTM Committee E04 on Metallog-
raphy and is the direct responsibility of Subcommittee E04.01 on Specimen
Preparation. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Oct. 1, 2012. Published October 2012. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 1990. Last previous edition approved in 2006 as E1351–01(2006). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/E1351-01R12. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1351 − 01 (2012)
NOTE 1—It is recommended that the purchaser of a field replication tester.Areplicamayalsobemadeonthedecarburizedsurface,ifitserves
service specify that each replicator demonstrate proficiency by providing the purpose of the investigation.
field prepared replica metallography and direct LM and SEM comparison
6.4 Do not remove any precipitates, carbides, nonmetallic
to laboratory prepared samples of an identical material by grade and
inclusions such as oxides and sulfides during the polishing or
service exposure.
etching operations.
5. Evaluation Methods
6.5 Etchingproceduresforsurfacemetallographicexamina-
5.1 A suitable replica should accurately reproduce all the
tion should be performed in accordance with Practice E407.
microstructural features present on the surface that was repli-
6.6 The quality of the surface preparation should be con-
cated.
trolled by the use of a portable field microscope.
5.2 No visible loss of resolution is permitted over the
6.7 To prevent possible contamination of any components,
normal range of magnifications on the LM as shown in Figs.
the etched area should be prepared carefully and thoroughly
1-3.
washed after replication.
5.3 The resolution of the structural detail in the replica
should exceed 0.1 µm to permit SEM examination at high
7. Replication Technique
magnifications (up to 5000×). See Figs. 4-6.
7.1 Ingeneral,areplicatedareaof12by18mm(0.5by0.75
in.) is satisfactory.
6. Metal Surface Preparation
7.2 A replica is produced by one of the two methods
6.1 If magnetic particle testing was previously used on the
described below. All methods produce acceptable replicas.
work-piece, demagnetize the piece before beginning surface
7.2.1 A replica may be produced by wetting one side of a
preparation.
sheet of plastic film with a suitable solvent, such as acetone or
6.2 Surfacepreparationmaybeaccomplishedusingmanual,
methyl acetate, and applying the wetted side of the film to the
mechanical, or electrolytic polishing methods.
prepared metal surface.
NOTE 2—Electrolytic preparation always carries the risk of pitting, and
7.2.2 Alternatively, a replica may be produced by wetting
of enlarging existing voids such as creep cavities and porosity.
the prepared metallic surface with a suitable solvent, such as
6.3 Prepare the surface to be replicated using the methods
acetoneormethylacetate,andapplyingthestripofplasticfilm
suggestedinMethodsE3modifiedforfielduse,asappropriate, (usually cellulose acetate) to the wet surface. The film is
in such a way as to obtain a surface free of deformation,
pressed against the surface for several seconds to ensure
scratches,polishingdefects,etchpits,andotherartifactswhich adherance.
may obscure the true microstructural features.
7.2.3 Apply a rubber-based replicating compound to the
preparedmetalsurface.Coverwiththematerial’scarrierpaper,
NOTE 3—The presence of decarburization can be detected with a
then use a roller to spread the compound into a uniformly thin
po
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