E04.01 - Specimen Preparation

SIGNIFICANCE AND USE
3.1 Applications of Macroetching:  
3.1.1 Macroetching is used to reveal the heterogeneity of metals and alloys. Metallographic specimens and chemical analyses will provide the necessary detailed information about specific localities, but they cannot give data about variation from one place to another unless an inordinate number of specimens are taken.  
3.1.2 Macroetching, on the other hand, will provide information on variations in (1) structure, such as grain size, flow lines, columnar structure, dendrites, and so forth; (2) variations in chemical composition as evidenced by segregation, carbide and ferrite banding, coring, inclusions, and depth of carburization or decarburization. The information provided about variations in chemical composition is strictly qualitative but the location of extremes in segregation will be shown. Chemical analyses or other means of determining the chemical composition would have to be performed to determine the extent of variation. Macroetching will also show the presence of discontinuities and voids, such as seams, laps, porosity, flakes, bursts, extrusion rupture, cracks, and so forth.  
3.1.3 Other applications of macroetching in the fabrication of metals are the study of weld structure, definition of weld penetration, dilution of filler metal by base metals, entrapment of flux, porosity, and cracks in weld and heat affected zones, and so forth. It is also used in the heat-treating shop to determine location of hard or soft spots, tong marks, quenching cracks, case depth in shallow-hardening steels, case depth in carburization, effectiveness of stop-off coatings in carburization, and so forth. In the machine shop, it can be used for the determination of grinding cracks in tools and dies.  
3.1.4 Macroetching is used extensively for quality control in the steel industry, to determine the tone of a heat in billets with respect to inclusions, segregation, and structure. Forge shops, in addition, use macroetching to reveal flow...
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1.1 These procedures describe the methods of macroetching metals and alloys to reveal their macrostructure.  
1.2 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to the International System (SI) units that are provided for information only and are not considered standard.  
1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
For specific warning statements, see 6.2, 7.1, 8.1.3, 8.2.1, 8.8.3, 8.10.1.1, and 8.13.2. It is further recommended to review the guidance in Guide E2014.  
1.4 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.

SIGNIFICANCE AND USE
5.1 This practice lists recommended methods and solutions for the etching of specimens for metallographic examination. Solutions are listed that highlight the phases and constituents present in most major alloy systems.
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1.1 This practice covers chemical solutions and procedures to be used in etching metals and alloys for microscopic examination. Safety precautions and miscellaneous information are also included.  
1.2 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific cautionary statements, see 6.1 and Table 2.  
1.3 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.

SIGNIFICANCE AND USE
4.1 Advantages of Electrolytic Polishing:  
4.1.1 For some metals, a high quality surface finish can be produced that is equivalent to, or better than, that which can be obtained by mechanical methods.  
4.1.2 Once procedures have been established, satisfactory results can be obtained rapidly with reproducibility.  
4.1.3 There can be a marked saving of time if many specimens of the same material are polished sequentially.  
4.1.4 Electropolishing a selected area on the surface of a relatively large metal part can be accomplished nondestructively, that is, without the need for sectioning to remove a piece.  
4.1.5 Soft, single-phase metals, which may be difficult to polish by mechanical methods, may be successfully electropolished.  
4.1.6 The true microstructure of a specimen can be obtained because artifacts (such as disturbed metal, scratches, and mechanical twins) produced on the surface, even by careful grinding and mechanical polishing operations, can be removed. These features are important in low-load hardness testing, X-ray diffraction studies, and in electron microscopy, where higher resolution puts a premium on undistorted metal surfaces.  
4.1.7 After electropolishing is completed, etching can often be accomplished by reducing the voltage (generally to about one-tenth that required for polishing) for a short time before it is turned off.
Note 2: Not all electropolishing solutions produce good etching results.  
4.2 Disadvantages of Electrolytic Polishing:  
4.2.1 Many of the chemical mixtures used in electropolishing are poisonous or dangerous if not properly handled (see Section 5). These hazards are similar to those involved in the mixing and handling of etchants, see Test Methods E407.  
4.2.2 In multi-phase alloys, the polishing rate of each phase may be different. The result may be a non-planar surface.  
4.2.3 Electropolished surfaces may be slightly undulated rather than perfectly planar and, therefore, may not be suitable for exami...
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1.1 This guide deals with electrolytic polishing as a means of preparation of specimens for metallographic purposes. Procedures are described for polishing a variety of metals.  
Note 1: References (1-133)2 on electrolytic polishing will provide the reader with specific information beyond the scope of this guide.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific safety precautions are described in Section 5 and 6.3.1.  
1.4 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.

SIGNIFICANCE AND USE
5.1 The sulfur print reveals the distribution of sulfur as sulfide inclusions in the specimen. The sulfur print complements macroetch methods by providing an additional procedure for evaluating the homogeneity of a steel product.  
5.2 Sulfur prints of as-cast specimens generally reveal the solidification pattern and may be used to assess the nature of deoxidation, that is, rimming action versus killed steel sulfur distributions.  
5.3 Sulfur prints will reveal segregation patterns, including refilled cracks, and may reveal certain physical irregularities, for example, porosity or cracking.  
5.4 The nature of metal flow, such as in various forging operations, can be revealed using sulfur prints of specimens cut parallel to the metal flow direction.  
5.5 The sulfur print method is suitable for process control, research and development studies, failure analysis, and for material acceptance purposes.  
5.6 The intensity of the sulfur print is influenced by the concentration of sulfur in the steel, the chemical composition of the sulfide inclusions, the aggressiveness of the aqueous acid solution, and the duration of the contact printing between the acid soaked emulsion coated paper and the ground surface of the specimen (this time is the order of seconds rather than minutes). Very low sulfur content steels will produce too faint an image to be useful for macrostructural evaluations. Selection of appropriate printing practices including selection of type of emulsion coated media, acid type and strength, will yield satisfactory prints. Very faint images in the sulfur print can be made more visible by scanning the sulfur print into a PC, and using a photo editor to increase the color saturation. Steels with compositions that produce predominantly titanium or chromium sulfides will not produce useful images.
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1.1 This practice provides information required to prepare sulfur prints (also referred to as Baumann Prints) of most ferrous alloys to reveal the distribution of sulfide inclusions.  
1.2 The sulfur print reveals the distribution of sulfides in steels with bulk sulfur contents between about 0.010 and 0.40 weight percent.  
1.3 Certain steels contain complex sulfides that do not respond to the test solutions, for example, steels containing titanium sulfides or chromium sulfides.  
1.4 The sulfur print test is a qualitative test. The density of the print image should not be used to assess the sulfur content of a steel. Under carefully controlled conditions, it is possible to compare print image intensities if the images are formed only by manganese sulfides.  
1.5 The sulfur print image will reveal details of the solidification pattern or metal flow from hot or cold working on appropriately chosen and prepared test specimens.  
1.6 This practice does not address acceptance criteria based on the use of the method.  
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.8 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific precautionary statements, see Section 9.  
1.9 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.

SIGNIFICANCE AND USE
4.1 One of the fundamental objectives of microstructural examination of manufactured materials, especially plastics and polymers, is to gain a more complete understanding of the relationships between the manufacturing processes, the microstructure and texture of the material, and the product's performance (that is, physical, optical, or mechanical properties, or combination thereof). Under nearly all conditions, the proper selection and preparation of the specimen are of major importance.  
4.2 Because of the wide range of available equipment; physical, chemical, and mechanical properties of materials; and the personal element, specimen preparation is an art based upon scientific principles. However, like metallographic specimen preparation, certain methods, practices, and procedures can be used to routinely produce acceptable quality plastic and polymeric specimens for microstructural examination. Acceptable quality means:  
4.2.1 The observed microstructure is free of thermal, mechanical, and chemical alterations, artifacts, damage, or defects resulting from the specimen preparation process.  
4.2.2 A surface finish appropriate for the microscopical techniques to be used.  
4.2.3 The microstructure is reproducibly displayed for a given specimen.  
4.3 The mounting, sectioning, grinding, and polishing procedures in this guide may introduce thermal, mechanical, and chemical stresses on the material being prepared for microstructural examination. Thus, knowledge of the material's physical, mechanical, and chemical properties is of importance in selecting the most appropriate technique(s) to reveal its true microstructure and to minimize the total number of steps needed to produce high quality polished specimens.  
4.4 The general guidelines presented below will need to be modified for each type of plastic or polymer to be prepared. Table X1.1 presents general procedures for preparing plastics and polymers. Tables X1.2-X1.5 present procedures for preparing four ...
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1.1 This guide covers recommended procedures and guidelines for the preparation of plastic and polymeric specimens for microstructural examination by light and electron microscopy.  
1.2 This guide is applicable to most semi-rigid and rigid plastics, including engineering plastics. This guide is also applicable to some non-rigid plastics.  
1.3 The procedures and guidelines presented in this guide are those which generally produce satisfactory specimens. This guide does not describe the variations in techniques required to solve individual problems.  
1.4 Many detailed descriptions of grinding and polishing of plastics and polymers are available (1-7).2  
1.5 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 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.

SIGNIFICANCE AND USE
4.1 TSCs are used in a number of critical industrial components. TSCs can be expected to contain measurable levels of porosity and linear detachment. Accurate and consistent evaluation of specimens is essential to ensure the integrity of the coating and proper adherence to the substrate.  
4.1.1 Example 1: By use of inappropriate metallographic methods, the apparent amount of porosity and linear detachment displayed by a given specimen can be increased, by excessive edge rounding, or decreased by smearing of material into voids. Therefore inaccurate levels of porosity and linear detachment will be reported even when the accuracy of the measurement technique is acceptable.  
4.1.2 Example 2: Inconsistent metallographic preparation methods can cause the apparent amount of voids to vary excessively indicating a poorly controlled thermal spray process, while the use of consistent practice will regularly display the true microstructure and verify the consistency of the thermal spray process.  
4.2 During the development of TSC procedures, metallographic information is necessary to validate the efficacy of a specific application.  
4.3 Cross sections are usually taken perpendicular to the long axis of the specimen and prepared to reveal information concerning the following:  
4.3.1 Variations in structure from surface to substrate,  
4.3.2 The distribution of unmelted particles throughout the coating,  
4.3.3 The distribution of linear detachment throughout the coating,  
4.3.4 The distribution of porosity throughout the coating,  
4.3.5 The presence of contamination within the coating,  
4.3.6 The thickness of the coating (top coat and bond coat, where applicable),  
4.3.7 The presence of interfacial contamination,  
4.3.8 The integrity of the interface between the coating and substrate, and,  
4.3.9 The integrity of the coating microstructure with respect to chemistry.
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1.1 This guide covers recommendations for sectioning, cleaning, mounting, grinding, and polishing to reveal the microstructural features of thermal sprayed coatings (TSCs) and the substrates to which they are applied when examined microscopically. Because of the diversity of available equipment, the wide variety of coating and substrate combinations, and the sensitivity of these specimens to preparation technique, the existence of a series of recommended methods for metallographic preparation of thermal sprayed coating specimens is helpful. Adherence to this guide will provide practitioners with consistent and reproducible results. Additional information concerning standard practices for metallographic preparation can be found in Guide E3.  
1.2 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.3 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.

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.
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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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
4.1 Inclusion ratings done either manually using Test Methods E45 or automatically using Practice E1122 or E1245 are influenced by the quality of specimen preparation. This guide provides examples of proven specimen preparation methods that retain inclusions in polished steel specimens.  
4.2 This guide provides a procedure to determine if the prepared specimens are of suitable quality for subsequent rating of inclusions. None of these methods should be construed as defining or establishing specific procedures or limits of acceptability for any steel grade.
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1.1 This guide2 covers two preparation methods for steel metallographic specimens that will be analyzed for nonmetallic inclusions with automatic image analysis (AIA) equipment. The two methods of preparation are offered as accepted methods used to retain nonmetallic inclusions in steel. This guide does not limit the user to these methods.  
1.2 A procedure to test the suitability of the prepared specimen for AIA inclusion work, using differential interference contrast (DIC), is presented.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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.

SIGNIFICANCE AND USE
4.1 This guide is intended as a summary of safety practices in the metallography laboratory. It can be used as a training reference for those new to the field of metallography and as a refresher to those who are experienced.  
4.2 This guide is not intended to be inclusive of all safety concerns encountered in a metallographic laboratory. Several books that provide safety information are available (1-15).5  
4.3 Before operating any equipment, it is advisable to read and understand the accompanying manuals and to follow any specified safety guidelines.  
4.4 Safety data sheets (SDS) for chemicals being used in a laboratory should be on file and readily accessible. When working with any chemicals, especially for the first time, one should review the SDS supplied by the manufacturer and follow any safety guidelines suggested. The most current and applicable SDS should be on file for a given product or chemical.
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1.1 This guide outlines the basic safety guidelines to be used in a metallographic laboratory. Safe working habits are discussed for various tasks performed in a metallographic laboratory.  
1.2 The sections appear in the following order:    
Section  
Scope  
1  
Referenced Documents  
2  
Terminology  
3  
Significance and Use  
4  
General  
5  
Heat Treating  
6  
Specimen Preparation/Sectioning  
7  
Specimen Mounting  
8  
Mechanical Grinding/Polishing  
9  
Chemical Safety  
10  
Electrolytic Polishing/Etching  
11  
Sulfur Printing  
12  
Laboratory Ventilation/Fume Hoods  
13  
Chemical Spills  
14  
Photography  
15  
X ray/Electron Microscopy  
16  
Laboratory Ergonomics  
17  
Disposal of Residues  
18  
Keywords  
19  
1.3 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.  
1.4 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.

SIGNIFICANCE AND USE
4.1 Microstructures have a strong influence on the properties and successful application of metals and alloys. Determination and control of microstructure requires the use of metallographic examination.  
4.2 Many specifications contain a requirement regarding microstructure; hence, a major use for metallographic examination is inspection to ensure that the requirement is met. Other major uses for metallographic examination are in failure analysis, and in research and development.  
4.3 Proper choice of specimen location and orientation will minimize the number of specimens required and simplify their interpretation. It is easy to take too few specimens for study, but it is seldom that too many are studied.
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1.1 The primary objective of metallographic examinations is to reveal the constituents and structure of metals and their alloys by means of a light optical or scanning electron microscope. In special cases, the objective of the examination may require the development of less detail than in other cases but, under nearly all conditions, the proper selection and preparation of the specimen is of major importance. Because of the diversity in available equipment and the wide variety of problems encountered, the following text presents for the guidance of the metallographer only those practices which experience has shown are generally satisfactory; it cannot and does not describe the variations in technique required to solve individual specimen preparation problems.  
Note 1: For a more extensive description of various metallographic techniques, refer to Samuels, L. E.,  Metallographic Polishing by Mechanical Methods, American Society for Metals (ASM) Metals Park, OH, 3rd Ed., 1982; Petzow, G.,  Metallographic Etching, ASM, 1978; and VanderVoort, G.,  Metallography: Principles and Practice, McGraw Hill, NY, 2nd Ed., 1999.  
1.2 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.  
1.3 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.

SIGNIFICANCE AND USE
5.1 This practice lists recommended methods and solutions for the etching of specimens for metallographic examination. Solutions are listed to highlight phases present in most major alloy systems.
SCOPE
1.1 This practice covers chemical solutions and procedures to be used in etching metals and alloys for microscopic examination. Safety precautions and miscellaneous information are also included.  
1.2 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. For specific cautionary statements, see 6.1 and Table 2.

SIGNIFICANCE AND USE
5.1 This practice lists recommended methods and solutions for the etching of specimens for metallographic examination. Solutions are listed to highlight phases present in most major alloy systems.
SCOPE
1.1 This practice covers chemical solutions and procedures to be used in etching metals and alloys for microscopic examination. Safety precautions and miscellaneous information are also included.  
1.2 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. For specific cautionary statements, see 6.1 and Table 2.

SIGNIFICANCE AND USE
3.1 Applications of Macroetching:  
3.1.1 Macroetching is used to reveal the heterogeneity of metals and alloys. Metallographic specimens and chemical analyses will provide the necessary detailed information about specific localities but they cannot give data about variation from one place to another unless an inordinate number of specimens are taken.  
3.1.2 Macroetching, on the other hand, will provide information on variations in (1) structure, such as grain size, flow lines, columnar structure, dendrites, and so forth; (2) variations in chemical composition as evidenced by segregation, carbide and ferrite banding, coring, inclusions, and depth of carburization or decarburization. The information provided about variations in chemical composition is strictly qualitative but the location of extremes in segregation will be shown. Chemical analyses or other means of determining the chemical composition would have to be performed to determine the extent of variation. Macroetching will also show the presence of discontinuities and voids, such as seams, laps, porosity, flakes, bursts, extrusion rupture, cracks, and so forth.  
3.1.3 Other applications of macroetching in the fabrication of metals are the study of weld structure, definition of weld penetration, dilution of filler metal by base metals, entrapment of flux, porosity, and cracks in weld and heat affected zones, and so forth. It is also used in the heat-treating shop to determine location of hard or soft spots, tong marks, quenching cracks, case depth in shallow-hardening steels, case depth in carburization of dies, effectiveness of stop-off coatings in carburization, and so forth. In the machine shop, it can be used for the determination of grinding cracks in tools and dies.  
3.1.4 Macroetching is used extensively for quality control in the steel industry, to determine the tone of a heat in billets with respect to inclusions, segregation, and structure. Forge shops, in addition, use macroetching to reve...
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1.1 These procedures describe the methods of macroetching metals and alloys to reveal their macrostructure.  
1.2 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.  
1.3 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. For specific warning statements, see 6.2, 7.1, 8.1.3, 8.2.1, 8.8.3, 8.10.1.1, and 8.13.2.

SIGNIFICANCE AND USE
4.1 One of the fundamental objectives of microstructural examination of manufactured materials, especially plastics and polymers, is to gain a more complete understanding of the relationships between the manufacturing processes, the microstructure and texture of the material, and the product's performance (that is, physical, optical, or mechanical properties, or combination thereof). Under nearly all conditions, the proper selection and preparation of the specimen are of major importance.  
4.2 Because of the wide range of available equipment; physical, chemical, and mechanical properties of materials; and the personal element, specimen preparation is an art based upon scientific principles. However, like metallographic specimen preparation, certain methods, practices, and procedures can be used to routinely produce acceptable quality plastic and polymeric specimens for microstructural examination. Acceptable quality means:  
4.2.1 The observed microstructure is free of thermal, mechanical, and chemical alterations, artifacts, damage, or defects resulting from the specimen preparation process.  
4.2.2 A surface finish appropriate for the microscopical techniques to be used.  
4.2.3 The microstructure is reproducibly displayed for a given specimen.  
4.3 The mounting, sectioning, grinding, and polishing procedures in this guide may introduce thermal, mechanical, and chemical stresses on the material being prepared for microstructural examination. Thus, knowledge of the material's physical, mechanical, and chemical properties is of importance in selecting the most appropriate technique(s) to reveal its true microstructure and to minimize the total number of steps needed to produce high quality polished specimens.  
4.4 The general guidelines presented below will need to be modified for each type of plastic or polymer to be prepared. Table X1.1 presents general procedures for preparing plastics and polymers. Tables X1.2-X1.5 present procedures for preparing four ...
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1.1 This guide covers recommended procedures and guidelines for the preparation of plastic and polymeric specimens for microstructural examination by light and electron microscopy.  
1.2 This guide is applicable to most semi-rigid and rigid plastics, including engineering plastics. This guide is also applicable to some non-rigid plastics.  
1.3 The procedures and guidelines presented in this guide are those which generally produce satisfactory specimens. This guide does not describe the variations in techniques required to solve individual problems.  
1.4 Many detailed descriptions of grinding and polishing of plastics and polymers are available (1-7).2  
1.5 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.

SIGNIFICANCE AND USE
5.1 The sulfur print reveals the distribution of sulfur as sulfide inclusions in the specimen. The sulfur print complements macroetch methods by providing an additional procedure for evaluating the homogeneity of a steel product.  
5.2 Sulfur prints of as-cast specimens generally reveal the solidification pattern and may be used to assess the nature of deoxidation, that is, rimming action versus killed steel sulfur distributions.  
5.3 Sulfur prints will reveal segregation patterns, including refilled cracks, and may reveal certain physical irregularities, for example, porosity or cracking.  
5.4 The nature of metal flow, such as in various forging operations, can be revealed using sulfur prints of specimens cut parallel to the metal flow direction.  
5.5 The sulfur print method is suitable for process control, research and development studies, failure analysis, and for material acceptance purposes.  
5.6 The intensity of the sulfur print is influenced by the concentration of sulfur in the steel, the chemical composition of the sulfide inclusions, the aggressiveness of the aqueous acid solution, and the duration of the contact printing between the acid soaked emulsion coated paper and the ground surface of the specimen (this time is the order of seconds rather than minutes). Very low sulfur content steels will produce too faint an image to be useful for macrostructural evaluations. Selection of appropriate printing practices including selection of type of emulsion coated media, acid type and strength, will yield satisfactory prints. Very faint images in the sulfur print can be made more visible by scanning the sulfur print into a PC, and using a photo editor to increase the color saturation. Steels with compositions that produce predominantly titanium or chromium sulfides will not produce useful images.
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1.1 This practice provides information required to prepare sulfur prints (also referred to as Baumann Prints) of most ferrous alloys to reveal the distribution of sulfide inclusions.  
1.2 The sulfur print reveals the distribution of sulfides in steels with bulk sulfur contents between about 0.010 and 0.40 weight percent.  
1.3 Certain steels contain complex sulfides that do not respond to the test solutions, for example, steels containing titanium sulfides or chromium sulfides.  
1.4 The sulfur print test is a qualitative test. The density of the print image should not be used to assess the sulfur content of a steel. Under carefully controlled conditions, it is possible to compare print image intensities if the images are formed only by manganese sulfides.  
1.5 The sulfur print image will reveal details of the solidification pattern or metal flow from hot or cold working on appropriately chosen and prepared test specimens.  
1.6 This practice does not address acceptance criteria based on the use of the method.  
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.8 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. For specific precautionary statements, see Section 9.

SIGNIFICANCE AND USE
4.1 Advantages of Electrolytic Polishing:  
4.1.1 For some metals, a high quality surface finish can be produced that is equivalent to, or better than, that which can be obtained by mechanical methods.  
4.1.2 Once procedures have been established, satisfactory results can be obtained rapidly with reproducibility.  
4.1.3 There can be a marked saving of time if many specimens of the same material are polished sequentially.  
4.1.4 Electropolishing a selected area on the surface of a relatively large metal part can be accomplished nondestructively, that is, without the need for sectioning to remove a piece.  
4.1.5 Soft, single-phase metals, which may be difficult to polish by mechanical methods, may be successfully electropolished.  
4.1.6 The true microstructure of a specimen can be obtained because artifacts (such as disturbed metal, scratches, and mechanical twins) produced on the surface, even by careful grinding and mechanical polishing operations, can be removed. These features are important in low-load hardness testing, X-ray diffraction studies, and in electron microscopy, where higher resolution puts a premium on undistorted metal surfaces.  
4.1.7 After electropolishing is completed, etching can often be accomplished by reducing the voltage (generally to about one-tenth that required for polishing) for a short time before it is turned off.
Note 2: Not all electropolishing solutions produce good etching results.  
4.2 Disadvantages of Electrolytic Polishing:  
4.2.1 Many of the chemical mixtures used in electropolishing are poisonous or dangerous if not properly handled (see Section 5). These hazards are similar to those involved in the mixing and handling of etchants, see Test Methods E407.  
4.2.2 In multi-phase alloys, the polishing rate of each phase may be different. The result may be a non-planar surface.  
4.2.3 Electropolished surfaces may be slightly undulated rather than perfectly planar and, therefore, may not be suitable for exami...
SCOPE
1.1 This guide deals with electrolytic polishing as a means of preparation of specimens for metallographic purposes. Procedures are described for polishing a variety of metals.  
Note 1: References (1-133)2 on electrolytic polishing will provide the reader with specific information beyond the scope of this guide.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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.  Specific safety precautions are described in Section 5 and 6.3.1.

SIGNIFICANCE AND USE
4.1 TSCs are used in a number of critical industrial components. TSCs can be expected to contain measurable levels of porosity and linear detachment. Accurate and consistent evaluation of specimens is essential to ensure the integrity of the coating and proper adherence to the substrate.  
4.1.1 Example 1: By use of inappropriate metallographic methods, the apparent amount of porosity and linear detachment displayed by a given specimen can be increased, by excessive edge rounding, or decreased by smearing of material into voids. Therefore inaccurate levels of porosity and linear detachment will be reported even when the accuracy of the measurement technique is acceptable.  
4.1.2 Example 2: Inconsistent metallographic preparation methods can cause the apparent amount of voids to vary excessively indicating a poorly controlled thermal spray process, while the use of consistent practice will regularly display the true microstructure and verify the consistency of the thermal spray process.  
4.2 During the development of TSC procedures, metallographic information is necessary to validate the efficacy of a specific application.  
4.3 Cross sections are usually taken perpendicular to the long axis of the specimen and prepared to reveal information concerning the following:  
4.3.1 Variations in structure from surface to substrate,  
4.3.2 The distribution of unmelted particles throughout the coating,  
4.3.3 The distribution of linear detachment throughout the coating,  
4.3.4 The distribution of porosity throughout the coating,  
4.3.5 The presence of contamination within the coating,  
4.3.6 The thickness of the coating (top coat and bond coat, where applicable),  
4.3.7 The presence of interfacial contamination,  
4.3.8 The integrity of the interface between the coating and substrate, and,  
4.3.9 The integrity of the coating microstructure with respect to chemistry.
SCOPE
1.1 This guide covers recommendations for sectioning, cleaning, mounting, grinding, and polishing to reveal the microstructural features of thermal sprayed coatings (TSCs) and the substrates to which they are applied when examined microscopically. Because of the diversity of available equipment, the wide variety of coating and substrate combinations, and the sensitivity of these specimens to preparation technique, the existence of a series of recommended methods for metallographic preparation of thermal sprayed coating specimens is helpful. Adherence to this guide will provide practitioners with consistent and reproducible results. Additional information concerning standard practices for metallographic preparation can be found in Practice E3.  
1.2 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.

SIGNIFICANCE AND USE
3.1 Applications of Macroetching :  
3.1.1 Macroetching is used to reveal the heterogeneity of metals and alloys. Metallographic specimens and chemical analyses will provide the necessary detailed information about specific localities but they cannot give data about variation from one place to another unless an inordinate number of specimens are taken.  
3.1.2 Macroetching, on the other hand, will provide information on variations in (1) structure, such as grain size, flow lines, columnar structure, dendrites, etc.; (2) variations in chemical composition as evidenced by segregation, carbide and ferrite banding, coring, inclusions, and depth of carburization or decarburization. The information provided about variations in chemical composition is strictly qualitative but the location of extremes in segregation will be shown. Chemical analyses or other means of determining the chemical composition would have to be performed to determine the extent of variation. Macroetching will also show the presence of discontinuities and voids, such as seams, laps, porosity, flakes, bursts, extrusion rupture, cracks, etc.  
3.1.3 Other applications of macroetching in the fabrication of metals are the study of weld structure, definition of weld penetration, dilution of filler metal by base metals, entrapment of flux, porosity, and cracks in weld and heat affected zones, etc. It is also used in the heat-treating shop to determine location of hard or soft spots, tong marks, quenching cracks, case depth in shallow-hardening steels, case depth in carburization of dies, effectiveness of stop-off coatings in carburization, etc. In the machine shop, it can be used for the determination of grinding cracks in tools and dies.  
3.1.4 Macroetching is used extensively for quality control in the steel industry, to determine the tone of a heat in billets with respect to inclusions, segregation, and structure. Forge shops, in addition, use macroetching to reveal flow lines in setting up the bes...
SCOPE
1.1 These test procedures describe the methods of macroetching metals and alloys to reveal their macrostructure.  
1.2 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.  
1.3 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. For specific warning statements, see 6.2, 7.1, 8.1.3, 8.2.1, 8.8.3, 8.10.1.1, and 8.13.2.

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.

SIGNIFICANCE AND USE
Microstructures have a strong influence on the properties and successful application of metals and alloys. Determination and control of microstructure requires the use of metallographic examination.
Many specifications contain a requirement regarding microstructure; hence, a major use for metallographic examination is inspection to ensure that the requirement is met. Other major uses for metallographic examination are in failure analysis, and in research and development.
Proper choice of specimen location and orientation will minimize the number of specimens required and simplify their interpretation. It is easy to take too few specimens for study, but it is seldom that too many are studied.
SCOPE
1.1 The primary objective of metallographic examinations is to reveal the constituents and structure of metals and their alloys by means of a light optical or scanning electron microscope. In special cases, the objective of the examination may require the development of less detail than in other cases but, under nearly all conditions, the proper selection and preparation of the specimen is of major importance. Because of the diversity in available equipment and the wide variety of problems encountered, the following text presents for the guidance of the metallographer only those practices which experience has shown are generally satisfactory; it cannot and does not describe the variations in technique required to solve individual specimen preparation problems.
Note 1—For a more extensive description of various metallographic techniques, refer to Samuels, L. E.,  Metallographic Polishing by Mechanical Methods, American Society for Metals (ASM) Metals Park, OH, 3rd Ed., 1982; Petzow, G.,  Metallographic Etching, ASM, 1978; and VanderVoort, G.,  Metallography: Principles and Practice, McGraw Hill, NY, 2nd Ed., 1999.  
1.2 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.

SIGNIFICANCE AND USE
4.1 Inclusion ratings done either manually using Test Methods E45 or automatically using Practice E1122 or E1245 are influenced by the quality of specimen preparation. This guide provides examples of proven specimen preparation methods that retain inclusions in polished steel specimens.  
4.2 This guide provides a procedure to determine if the prepared specimens are of suitable quality for subsequent rating of inclusions. None of these methods should be construed as defining or establishing specific procedures or limits of acceptability for any steel grade.
SCOPE
1.1 This guide2 covers two preparation methods for steel metallographic specimens that will be analyzed for nonmetallic inclusions with automatic image analysis (AIA) equipment. The two methods of preparation are offered as accepted methods used to retain nonmetallic inclusions in steel. This guide does not limit the user to these methods.  
1.2 A procedure to test the suitability of the prepared specimen for AIA inclusion work, using differential interference contrast (DIC), is presented.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.

SIGNIFICANCE AND USE
Inclusion ratings done either manually using Test Methods E45 or automatically using Practice E1122 or E1245 are influenced by the quality of specimen preparation. This guide provides examples of proven specimen preparation methods that retain inclusions in polished steel specimens.
This guide provides a procedure to determine if the prepared specimens are of suitable quality for subsequent rating of inclusions. None of these methods should be construed as defining or establishing specific procedures or limits of acceptability for any steel grade.
SCOPE
1.1 This guide covers two preparation methods for steel metallographic specimens that will be analyzed for nonmetallic inclusions with automatic image analysis (AIA) equipment. The two methods of preparation are offered as accepted methods used to retain nonmetallic inclusions in steel. This guide does not limit the user to these methods.  
1.2 A procedure to test the suitability of the prepared specimen for AIA inclusion work, using differential interference contrast (DIC), is presented.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.

SIGNIFICANCE AND USE
One of the fundamental objectives of microstructural examination of manufactured materials, especially plastics and polymers, is to gain a more complete understanding of the relationships between the manufacturing processes, the microstructure and texture of the material, and the product's performance (that is, physical, optical, or mechanical properties, or combination thereof). Under nearly all conditions, the proper selection and preparation of the specimen are of major importance.
Because of the wide range of available equipment; physical, chemical, and mechanical properties of materials; and the personal element, specimen preparation is an art based upon scientific principles. However, like metallographic specimen preparation, certain methods, practices, and procedures can be used to routinely produce acceptable quality plastic and polymeric specimens for microstructural examination. Acceptable quality means:
The observed microstructure is free of thermal, mechanical, and chemical alterations, artifacts, damage, or defects resulting from the specimen preparation process.
A surface finish appropriate for the microscopical techniques to be used.
The microstructure is reproducibly displayed for a given specimen.
The mounting, sectioning, grinding, and polishing procedures in this guide may introduce thermal, mechanical, and chemical stresses on the material being prepared for microstructural examination. Thus, knowledge of the material's physical, mechanical, and chemical properties is of importance in selecting the most appropriate technique(s) to reveal its true microstructure and to minimize the total number of steps needed to produce high quality polished specimens.
The general guidelines presented below will need to be modified for each type of plastic or polymer to be prepared. Table X1.1 presents general procedures for preparing plastics and polymers. Tables X1.2-X1.5 present procedures for preparing four polymers with very different mechanical ...
SCOPE
1.1 This guide covers recommended procedures and guidelines for the preparation of plastic and polymeric specimens for microstructural examination by light and electron microscopy.
1.2 This guide is applicable to most semi-rigid and rigid plastics, including engineering plastics. This guide is also applicable to some non-rigid plastics.
1.3 The procedures and guidelines presented in this guide are those which generally produce satisfactory specimens. This guide does not describe the variations in techniques required to solve individual problems.
1.4 Many detailed descriptions of grinding and polishing of plastics and polymers are available (1-7).  
1.5 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.

SIGNIFICANCE AND USE
Advantages of Electrolytic Polishing:  
For some metals, a high quality surface finish can be produced that is equivalent to, or better than, that which can be obtained by mechanical methods.
Once procedures have been established, satisfactory results can be obtained rapidly with reproducibility.
There can be a marked saving of time if many specimens of the same material are polished sequentially.
Electropolishing a selected area on the surface of a relatively large metal part can be accomplished nondestructively, that is, without the need for sectioning to remove a piece.
Soft, single-phase metals, which may be difficult to polish by mechanical methods, may be successfully electropolished.
The true microstructure of a specimen can be obtained because artifacts (such as disturbed metal, scratches, and mechanical twins) produced on the surface, even by careful grinding and mechanical polishing operations, can be removed. These features are important in low-load hardness testing, X-ray diffraction studies, and in electron microscopy, where higher resolution puts a premium on undistorted metal surfaces.
After electropolishing is completed, etching can often be accomplished by reducing the voltage (generally to about one-tenth that required for polishing) for a short time before it is turned off.
Note 2—Not all electropolishing solutions produce good etching results.
Disadvantages of Electrolytic Polishing:  
Many of the chemical mixtures used in electropolishing are poisonous or dangerous if not properly handled (see Section 5). These hazards are similar to those involved in the mixing and handling of etchants, see Test Methods E 407.
In multi-phase alloys, the polishing rate of each phase may be different. The result may be a non-planar surface.
Electropolished surfaces may be slightly undulated rather than perfectly planar and, therefore, may not be suitable for examination at all magnifications.
The rate of polishing in areas adjacent to var...
SCOPE
1.1 This guide deals with electrolytic polishing as a means of preparation of specimens for metallographic purposes. Procedures are described for polishing a variety of metals.
Note 1—References (1-133) on electrolytic polishing will provide the reader with specific information beyond the scope of this guide.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.  Specific safety precautions are described in Section 5 and 6.3.1.

SIGNIFICANCE AND USE
The sulfur print reveals the distribution of sulfur as sulfide inclusions in the specimen. The sulfur print complements macroetch methods by providing an additional procedure for evaluating the homogeneity of a steel product.
Sulfur prints of as-cast specimens generally reveal the solidification pattern and may be used to assess the nature of deoxidation, that is, rimming action versus killed steel sulfur distributions.
Sulfur prints will reveal segregation patterns, including refilled cracks, and may reveal certain physical irregularities, for example, porosity or cracking.
The nature of metal flow, such as in various forging operations, can be revealed using sulfur prints of specimens cut parallel to the metal flow direction.
The sulfur print method is suitable for process control, research and development studies, failure analysis, and for material acceptance purposes.
The intensity of the sulfur print is influenced by the concentration of sulfur in the steel, the chemical composition of the sulfide inclusions, the aggressiveness of the aqueous acid solution, and the duration of the contact printing between the acid soaked emulsion coated paper and the ground surface of the specimen (this time is the order of seconds rather than minutes). Very low sulfur content steels will produce too faint an image to be useful for macrostructural evaluations. Selection of appropriate printing practices including selection of type of emulsion coated media, acid type and strength, will yield satisfactory prints. Very faint images in the sulfur print can be made more visible by scanning the sulfur print into a PC, and using a photo editor to increase the color saturation. Steels with compositions that produce predominantly titanium or chromium sulfides will not produce useful images.
SCOPE
1.1 This practice provides information required to prepare sulfur prints (also referred to as Baumann Prints) of most ferrous alloys to reveal the distribution of sulfide inclusions.
1.2 The sulfur print reveals the distribution of sulfides in steels with bulk sulfur contents between about 0.010 and 0.40 weight percent.  
1.3 Certain steels contain complex sulfides that do not respond to the test solutions, for example, steels containing titanium sulfides or chromium sulfides.
1.4 The sulfur print test is a qualitative test. The density of the print image should not be used to assess the sulfur content of a steel. Under carefully controlled conditions, it is possible to compare print image intensities if the images are formed only by manganese sulfides.  
1.5 The sulfur print image will reveal details of the solidification pattern or metal flow from hot or cold working on appropriately chosen and prepared test specimens.
1.6 This practice does not address acceptance criteria based on the use of the method.
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.8 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. For specific precautionary statements, see Section 9.

SIGNIFICANCE AND USE
TSCs are used in a number of critical industrial components. TSCs can be expected to contain measurable levels of porosity and linear detachment. Accurate and consistent evaluation of specimens is essential to ensure the integrity of the coating and proper adherence to the substrate.
Example 1: By use of inappropriate metallographic methods, the apparent amount of porosity and linear detachment displayed by a given specimen can be increased, by excessive edge rounding, or decreased by smearing of material into voids. Therefore inaccurate levels of porosity and linear detachment will be reported even when the accuracy of the measurement technique is acceptable.
Example 2: Inconsistent metallographic preparation methods can cause the apparent amount of voids to vary excessively indicating a poorly controlled thermal spray process, while the use of consistent practice will regularly display the true microstructure and verify the consistency of the thermal spray process.
During the development of TSC procedures, metallographic information is necessary to validate the efficacy of a specific application.
Cross sections are usually taken perpendicular to the long axis of the specimen and prepared to reveal information concerning the following:
Variations in structure from surface to substrate,
The distribution of unmelted particles throughout the coating,
The distribution of linear detachment throughout the coating,
The distribution of porosity throughout the coating,
The presence of contamination within the coating,
The thickness of the coating (top coat and bond coat, where applicable),
The presence of interfacial contamination,
The integrity of the interface between the coating and substrate, and,
The integrity of the coating microstructure with respect to chemistry.
SCOPE
1.1 This guide covers recommendations for sectioning, cleaning, mounting, grinding, and polishing to reveal the microstructural features of thermal sprayed coatings (TSCs) and the substrates to which they are applied when examined microscopically. Because of the diversity of available equipment, the wide variety of coating and substrate combinations, and the sensitivity of these specimens to preparation technique, the existence of a series of recommended methods for metallographic preparation of thermal sprayed coating specimens is helpful. Adherence to this guide will provide practitioners with consistent and reproducible results. Additional information concerning standard practices for metallographic preparation can be found in Practice E 3.
1.2 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.

SIGNIFICANCE AND USE
Microstructures have a strong influence on the properties and successful application of metals and alloys. Determination and control of microstructure requires the use of metallographic examination.
Many specifications contain a requirement regarding microstructure; hence, a major use for metallographic examination is inspection to ensure that the requirement is met. Other major uses for metallographic examination are in failure analysis, and in research and development.
Proper choice of specimen location and orientation will minimize the number of specimens required and simplify their interpretation. It is easy to take too few specimens for study, but it is seldom that too many are studied.
SCOPE
1.1 The primary objective of metallographic examinations is to reveal the constituents and structure of metals and their alloys by means of a light optical or scanning electron microscope. In special cases, the objective of the examination may require the development of less detail than in other cases but, under nearly all conditions, the proper selection and preparation of the specimen is of major importance. Because of the diversity in available equipment and the wide variety of problems encountered, the following text presents for the guidance of the metallographer only those practices which experience has shown are generally satisfactory; it cannot and does not describe the variations in technique required to solve individual specimen preparation problems.
Note 1—For a more extensive description of various metallographic techniques, refer to Samuels, L. E.,  Metallographic Polishing by Mechanical Methods, American Society for Metals (ASM) Metals Park, OH, 3rd Ed., 1982; Petzow, G.,  Metallographic Etching, ASM, 1978; and VanderVoort, G.,  Metallography: Principles and Practice, McGraw Hill, NY, 2nd Ed., 1999.  
1.2 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.

SIGNIFICANCE AND USE
Microstructures have a strong influence on the properties and successful application of metals and alloys. Determination and control of microstructure requires the use of metallographic examination.
Many specifications contain a requirement regarding microstructure; hence, a major use for metallographic examination is inspection to ensure that the requirement is met. Other major uses for metallographic examination are in failure analysis, and in research and development.
Proper choice of specimen location and orientation will minimize the number of specimens required and simplify their interpretation. It is easy to take too few specimens for study, but it is seldom that too many are studied.
SCOPE
1.1 The primary objective of metallographic examinations is to reveal the constituents and structure of metals and their alloys by means of a light optical or scanning electron microscope. In special cases, the objective of the examination may require the development of less detail than in other cases but, under nearly all conditions, the proper selection and preparation of the specimen is of major importance. Because of the diversity in available equipment and the wide variety of problems encountered, the following text presents for the guidance of the metallographer only those practices which experience has shown are generally satisfactory; it cannot and does not describe the variations in technique required to solve individual specimen preparation problems.
Note 1 - For a more extensive description of various metallographic techniques, refer to Samuels, L. E.,  Metallographic Polishing by Mechanical Methods, American Society for Metals (ASM) Metals Park, OH, 3rd Ed., 1982; Petzow, G.,  Metallographic Etching, ASM, 1978; and VanderVoort, G.,  Metallography: Principles and Practice, McGraw Hill, NY, 2nd Ed., 1999.
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.

SIGNIFICANCE AND USE
This practice lists recommended methods and solutions for the etching of specimens for metallographic examination. Solutions are listed to highlight phases present in most major alloy systems.
SCOPE
1.1 This practice covers chemical solutions and procedures to be used in etching metals and alloys for microscopic examination. Safety precautions and miscellaneous information are also included.
1.2 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. For specific cautionary statements, see 6.1 and Table 2.

SIGNIFICANCE AND USE
This practice lists recommended methods and solutions for the etching of specimens for metallographic examination. Solutions are listed to highlight phases present in most major alloy systems.
SCOPE
1.1 This practice covers chemical solutions and procedures to be used in etching metals and alloys for microscopic examination. Safety precautions and miscellaneous information are also included.
1.2 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. For specific cautionary statements, see 6.1 and Table 2.

SIGNIFICANCE AND USE
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.
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.

SCOPE
1.1 These test procedures describe the methods of macro- etching metals and alloys to reveal their macrostructure.  
1.2 The values stated in inch-pound units are to be regarded as the standard. The SI equivalents of inch-pound units may be approximate.  
1.3 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.  For specific warning statements, see 6.2, 7.1, 8.1.3, 8.2.1, 8.8.3, 8.10.1.1, and 8.13.2.

SCOPE
1.1 Macroetching, which is the etching of specimens for macrostructural examination at low magnifications, is a frequently used technique for evaluating steel products such as bars, billets, blooms, and forgings.
1.2 Included in this method is a procedure for rating steel specimens by a graded series of photographs showing the incidence of certain conditions. The method is limited in application to bars, billets, blooms, and forgings of carbon and low alloy steels.
1.3 A number of different etching reagents may be used depending upon the type of examination to be made. Steels react differently to etching reagents because of variations in chemical composition, method of manufacture, heat treatment and many other variables. Establishment of general standards for acceptance or rejection for all conditions is impractical as some conditions must be considered relative to the part in which it occurs.
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. See the specific precautionary statement in 5.3.

SIGNIFICANCE AND USE
Inclusion ratings done either manually using Test Methods E 45 or automatically using Practice E 1122 or E 1245 are influenced by the quality of specimen preparation. This guide provides examples of proven specimen preparation methods that retain inclusions in polished steel specimens.
This guide provides a procedure to determine if the prepared specimens are of suitable quality for subsequent rating of inclusions. None of these methods should be construed as defining or establishing specific procedures or limits of acceptability for any steel grade.
SCOPE
1.1 This guide² covers two preparation methods for steel metallographic specimens that will be analyzed for nonmetallic inclusions with automatic image analysis (AIA) equipment. The two methods of preparation are offered as accepted methods used to retain nonmetallic inclusions in steel. This guide does not limit the user to these methods.
1.2 A procedure to test the suitability of the prepared specimen for AIA inclusion work, using differential interference contrast (DIC), is presented.

SCOPE
1.1 This guide covers two preparation methods for steel metallographic specimens that will be analyzed for nonmetallic inclusions with automatic image analysis (AIA) equipment. The two methods of preparation are offered as accepted methods used to retain nonmetallic inclusions in steel. This guide does not limit the user to these methods.
1.2 A procedure to test the suitability of the prepared specimen for AIA inclusion work, using differential interference contrast (DIC), is presented.

SIGNIFICANCE AND USE
One of the fundamental objectives of microstructural examination of manufactured materials, especially plastics and polymers, is to gain a more complete understanding of the relationships between the manufacturing processes, the microstructure and texture of the material, and the product’performance (that is, physical, optical, or mechanical properties, or combination thereof). Under nearly all conditions, the proper selection and preparation of the specimen are of major importance.
Because of the wide range of available equipment; physical, chemical, and mechanical properties of materials; and the personal element, specimen preparation is an art based upon scientific principles. However, like metallographic specimen preparation, certain methods, practices, and procedures can be used to routinely produce acceptable quality plastic and polymeric specimens for microstructural examination. Acceptable quality means:
4.2.1 The observed microstructure is free of thermal, mechanical, and chemical alterations, artifacts, damage, or defects resulting from the specimen preparation process.
4.2.2 A surface finish appropriate for the microscopical techniques to be used.
4.2.3 The microstructure is reproducibly displayed for a given specimen.
The mounting, sectioning, grinding, and polishing procedures in this guide may introduce thermal, mechanical, and chemical stresses on the material being prepared for microstructural examination. Thus, knowledge of the material’physical, mechanical, and chemical properties is of importance in selecting the most appropriate technique(s) to reveal its true microstructure and to minimize the total number of steps needed to produce high quality polished specimens.
The general guidelines presented below will need to be modified for each type of plastic or polymer to be prepared. Table X1.1 presents general procedures for preparing plastics and polymers. Tables X1.2-X1.5 present procedures for preparing four polymers with very differe...
SCOPE
1.1 This guide covers recommended procedures and guidelines for the preparation of plastic and polymeric specimens for microstructural examination by light and electron microscopy.
1.2 This guide is applicable to most semi-rigid and rigid plastics, including engineering plastics. This guide is also applicable to some non-rigid plastics.
1.3 The procedures and guidelines presented in this guide are those which generally produce satisfactory specimens. This guide does not describe the variations in techniques required to solve individual problems.
1.4 Many detailed descriptions of grinding and polishing of plastics and polymers are available (1-7).
1.5 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.

SCOPE
1.1 This guide deals with electrolytic polishing as a means of preparation of specimens for metallographic purposes. Procedures are described for polishing a variety of metals.
Note 1—References (1-133) on electrolytic polishing will provide the reader with specific information beyond the scope of this guide.
1.2 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. Specific safety precautions are described in Section 5 and 6.3.1.

SCOPE
1.1 This practice provides information required to prepare sulfur prints (also referred to as Baumann Prints) of most ferrous alloys to reveal the distribution of sulfide inclusions.
1.2 The sulfur print reveals the distribution of sulfides in steels with bulk sulfur contents between about 0.002 and 0.40 weight percent.
1.3 Certain steels contain complex sulfides that do not respond to the test solutions, for example, steels containing titanium sulfides or chromium sulfides.
1.4 The sulfur print test is a qualitative test. The density of the print image should not be used to assess the sulfur content of a steel. Under carefully controlled conditions, it is possible to compare print image intensities if the images are formed only by manganese sulfides.
1.5 The sulfur print image will reveal details of the solidification pattern or metal flow from hot or cold working on appropriately chosen and prepared test specimens.
1.6 This practice does not address acceptance criteria based on the use of the method.
1.7 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. For specific precautionary statements, see Section 9.

SIGNIFICANCE AND USE
The sulfur print reveals the distribution of sulfur as sulfide inclusions in the specimen. The sulfur print complements macroetch methods by providing an additional procedure for evaluating the homogeneity of a steel product.
Sulfur prints of as-cast specimens generally reveal the solidification pattern and may be used to assess the nature of deoxidation, that is, rimming action versus killed steel sulfur distributions.
Sulfur prints will reveal segregation patterns, including refilled cracks, and may reveal certain physical irregularities, for example, porosity or cracking.
The nature of metal flow, such as in various forging operations, can be revealed using sulfur prints of specimens cut parallel to the metal flow direction.
The sulfur print method is suitable for process control, research and development studies, failure analysis, and for material acceptance purposes.
The intensity of the sulfur print is influenced by the concentration of sulfur in the steel, the chemical composition of the sulfide inclusions, the aggressiveness of the aqueous acid solution, and the duration of the contact printing between the acid soaked emulsion coated paper and the ground surface of the specimen (this time is the order of seconds rather than minutes). Very low sulfur content steels will produce too faint an image to be useful for macrostructural evaluations. Selection of appropriate printing practices including selection of type of emulsion coated media, acid type and strength, will yield satisfactory prints. Very faint images in the sulfur print can be made more visible by scanning the sulfur print into a PC, and using a photo editor to increase the color saturation. Steels with compositions that produce predominantly titanium or chromium sulfides will not produce useful images.
SCOPE
1.1 This practice provides information required to prepare sulfur prints (also referred to as Baumann Prints) of most ferrous alloys to reveal the distribution of sulfide inclusions.
1.2 The sulfur print reveals the distribution of sulfides in steels with bulk sulfur contents between about 0.002 and 0.40 weight percent.
1.3 Certain steels contain complex sulfides that do not respond to the test solutions, for example, steels containing titanium sulfides or chromium sulfides.
1.4 The sulfur print test is a qualitative test. The density of the print image should not be used to assess the sulfur content of a steel. Under carefully controlled conditions, it is possible to compare print image intensities if the images are formed only by manganese sulfides.
1.5 The sulfur print image will reveal details of the solidification pattern or metal flow from hot or cold working on appropriately chosen and prepared test specimens.
1.6 This practice does not address acceptance criteria based on the use of the method.
1.7 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. For specific precautionary statements, see Section 9.

SIGNIFICANCE AND USE
TSCs are used in a number of critical industrial components. TSCs can be expected to contain measurable levels of porosity and linear detachment. Accurate and consistent evaluation of specimens is essential to ensure the integrity of the coating and proper adherence to the substrate.
4.1.1 Example 1: By use of inappropriate metallographic methods, the apparent amount of porosity and linear detachment displayed by a given specimen can be increased, by excessive edge rounding, or decreased by smearing of material into voids. Therefore inaccurate levels of porosity and linear detachment will be reported even when the accuracy of the measurement technique is acceptable.
4.1.2 Example 2: Inconsistent metallographic preparation methods can cause the apparent amount of voids to vary excessively indicating a poorly controlled thermal spray process, while the use of consistent practice will regularly display the true microstructure and verify the consistency of the thermal spray process.
During the development of TSC procedures, metallographic information is necessary to validate the efficacy of a specific application.
Cross sections are usually taken perpendicular to the long axis of the specimen and prepared to reveal information concerning the following:
4.3.1 Variations in structure from surface to substrate,
4.3.2 The distribution of unmelted particles throughout the coating,
4.3.3 The distribution of linear detachment throughout the coating,
4.3.4 The distribution of porosity throughout the coating,
4.3.5 The presence of contamination within the coating,
4.3.6 The thickness of the coating (top coat and bond coat, where applicable),
4.3.7 The presence of interfacial contamination,
4.3.8 The integrity of the interface between the coating and substrate, and,
4.3.9 The integrity of the coating microstructure with respect to chemistry.
SCOPE
1.1 This guide covers recommendations for sectioning, cleaning, mounting, grinding, and polishing to reveal the microstructural features of thermal sprayed coatings (TSCs) and the substrates to which they are applied when examined microscopically. Because of the diversity of available equipment, the wide variety of coating and substrate combinations, and the sensitivity of these specimens to preparation technique, the existence of a series of recommended methods for metallographic preparation of thermal sprayed coating specimens is helpful. Adherence to this guide will provide practitioners with consistent and reproducible results. Additional information concerning standard practices for metallographic preparation can be found in Practice E3.  
This standards 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.

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 the metallographic replica 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.

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 the metallographic replica 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.

SCOPE
1.1 Macroetching, which is the etching of specimens for macrostructural examination at low magnifications, is a frequently used technique for evaluating steel products such as bars, billets, blooms, and forgings.
1.2 Included in this method is a procedure for rating steel specimens by a graded series of photographs showing the incidence of certain conditions. The method is limited in application to bars, billets, blooms, and forgings of carbon and low alloy steels.
1.3 A number of different etching reagents may be used depending upon the type of examination to be made. Steels react differently to etching reagents because of variations in chemical composition, method of manufacture, heat treatment and many other variables. Establishment of general standards for acceptance or rejection for all conditions is impractical as some conditions must be considered relative to the part in which it occurs.
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. See the specific precautionary statement in 5.3.

SCOPE
1.1 The primary objective of metallographic examinations is to reveal the constituents and structure of metals and their alloys by means of a light optical or scanning electron microscope. In special cases, the objective of the examination may require the development of less detail than in other cases but, under nearly all conditions, the proper selection and preparation of the specimen is of major importance. Because of the diversity in available equipment and the wide variety of problems encountered, the following text presents for the guidance of the metallographer only those practices which experience has shown are generally satisfactory; it cannot and does not describe the variations in technique required to solve individual specimen preparation problems.
Note 1--For a more extensive description of various metallographic techniques, refer to Samuels, L. E.,  Metallographic Polishing by Mechanical Methods, American Society for Metals (ASM) Metals Park, OH, 3rd Ed., 1982; Petzow, G.,  Metallographic Etching, ASM, 1978; and VanderVoort, G., Metallography: Principles and Practice, McGraw Hill, NY, 2nd Ed., 1999.
1.2 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.

SCOPE
1.1 Macroetching, which is the etching of specimens for macrostructural examination at low magnifications, is a frequently used technique for evaluating steel products such as bars, billets, blooms, and forgings.
1.2 Included in this method is a procedure for rating steel specimens by a graded series of photographs showing the incidence of certain conditions. The method is limited in application to bars, billets, blooms, and forgings of carbon and low alloy steels.
1.3 A number of different etching reagents may be used depending upon the type of examination to be made. Steels react differently to etching reagents because of variations in chemical composition, method of manufacture, heat treatment and many other variables. Establishment of general standards for acceptance or rejection for all conditions is impractical as some conditions must be considered relative to the part in which it occurs.
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. See the specific precautionary statement in 5.3.

SCOPE
1.1 The primary objective of metallographic examinations is to reveal the constituents and structure of metals and their alloys by means of a light optical or scanning electron microscope. In special cases, the objective of the examination may require the development of less detail than in other cases but, under nearly all conditions, the proper selection and preparation of the specimen is of major importance. Because of the diversity in available equipment and the wide variety of problems encountered, the following text presents for the guidance of the metallographer only those practices which experience has shown are generally satisfactory; it cannot and does not describe the variations in technique required to solve individual specimen preparation problems.
Note 1--For a more extensive description of various metallographic techniques, refer to Samuels, L. E.,  Metallographic Polishing by Mechanical Methods, American Society for Metals (ASM) Metals Park, OH, 3rd Ed., 1982; Petzow, G.,  Metallographic Etching, ASM, 1978; and VanderVoort, G., Metallography: Principles and Practice, McGraw Hill, NY, 2nd Ed., 1999.
1.2 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.

SCOPE
1.1 These test procedures describe the methods of macro- etching metals and alloys to reveal their macrostructure.  
1.2 The values stated in inch-pound units are to be regarded as the standard. The SI equivalents of inch-pound units may be approximate.  
1.3 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.  For specific warning statements, see 6.2, 7.1, 8.1.3, 8.2.1, 8.8.3, 8.10.1.1, and 8.13.2.

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1.1 This guide deals with electrolytic polishing as a means of preparation of specimens for metallographic purposes. Procedures are described for polishing a variety of metals.  Note 1-References (1-133)  on electrolytic polishing will provide the reader with specific information beyond the scope of this guide.
1.2 This standard does not purport to address all of the safety problems, 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. Specific safety precautions are described in Section 5 and 6.3.1.

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1.1 This practice covers chemical solutions and procedures to be used in etching metals and alloys for microscopic examination. Safety precautions and miscellaneous information are also included.
1.2 This standard does not purport to address all of the safety problems, 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. For specific cautionary statements, see 6.1 and Table 2.

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1.1 This guide covers recommended procedures and guidelines for the preparation of plastic and polymeric specimens for microstructural examination by light and electron microscopy.
1.2 This guide is applicable to most semi-rigid and rigid plastics, including engineering plastics. This guide is also applicable to some non-rigid plastics.
1.3 The procedures and guidelines presented in this guide are those which generally produce satisfactory specimens. This guide does not describe the variations in techniques required to solve individual problems.
1.4 Many detailed descriptions of grinding and polishing of plastics and polymers are available (1-7).
1.5 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.