E04 - Metallography

SIGNIFICANCE AND USE
3.1 Pole figures are two-dimensional graphic representations, on polar coordinate paper, of the average distribution of crystallite orientations in three dimensions. Data for constructing pole figures are obtained with X-ray diffractometers, using reflection and transmission techniques.  
3.2 Several alternative procedures may be used. Some produce complete pole figures. Others yield partial pole figures, which may be combined to produce a complete figure.
SCOPE
1.1 This test method covers the use of the X-ray diffractometer to prepare quantitative pole figures.  
1.2 The test method consists of several experimental procedures. Some of the procedures (1-5)2 permit preparation of a complete pole figure. Others must be used in combination to produce a complete pole figure.  
1.3 Pole figures (6)  and inverse pole figures (7-10)  are two dimensional averages of the three-dimensional crystallite orientation distribution. Pole figures may be used to construct either inverse pole figures (11-13)  or the crystallite orientation distribution (14-21). Development of series expansions of the crystallite orientation distribution from reflection pole figures (22, 23)  makes it possible to obtain a series expansion of a complete pole figure from several incomplete pole figures. Pole figures or inverse pole figures derived by such methods shall be termed calculated. These techniques will not be described herein.  
1.4 Provided the orientation is homogeneous through the thickness of the sheet, certain procedures  (1-3)  may be used to obtain a complete pole figure.  
1.5 Provided the orientation has mirror symmetry with respect to planes perpendicular to the rolling, transverse, and normal directions, certain procedures (4, 5, 24)  may be used to obtain a complete pole figure.  
1.6 The test method emphasizes the Schulz reflection technique (25).  Other techniques (3, 4, 5, 24)  may be considered variants of the Schulz technique and are cited as options, but not described herein.  
1.7 The test method also includes a description of the transmission technique of Decker, et al (26),  which may be used in conjunction with the Schulz reflection technique to obtain a complete pole figure.  
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.  
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 The traditional resolution test of the SEM requires, as a first step, a photomicrograph of a fine particulate sample taken at a high magnification. The operator is required to measure a distance on the photomicrograph between two adjacent, but separate edges. These edges are usually less than one millimetre apart. Their image quality is often less than optimum limited by the S/N ratio of a beam with such a small diameter and low current. Operator judgment is dependent on the individual acuity of the person making the measurement and can vary significantly.  
4.2 Use of this practice results in SEM electron beam size characterization which is significantly more reproducible than the traditional resolution test using a fine particulate sample.
SCOPE
1.1 This practice provides a reproducible means by which one aspect of the performance of a scanning electron microscope (SEM) may be characterized. The resolution of an SEM depends on many factors, some of which are electron beam voltage and current, lens aberrations, contrast in the specimen, and operator-instrument-material interaction. However, the resolution for any set of conditions is limited by the size of the electron beam. This size can be quantified through the measurement of an effective apparent edge sharpness for a number of materials, two of which are suggested. This practice requires an SEM with the capability to perform line-scan traces, for example, Y-deflection waveform generation, for the suggested materials. The range of SEM magnification at which this practice is of utility is from 1000 × to 50 000 × . Higher magnifications may be attempted, but difficulty in making precise measurements can be expected.  
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 This guide is useful for the photomicrography and photomacrography of metals and other materials.  
4.2 The subsequent processing of the photographic materials is also treated.
SCOPE
1.1 This guide outlines various methods which may be followed in the photography of metals and materials with the reflected-light microscope. Methods are included for preparation of prints and transparencies in black-and-white and in color, using both direct rapid and wet processes.  
1.2 Guidelines are suggested to yield photomicrographs of typical subjects and, to the extent possible, of atypical subjects as well. Information is included concerning techniques for the enhanced display of specific material features. Descriptive material is provided where necessary to clarify procedures. References are cited where detailed descriptions may be helpful.  
1.3 The sections appear in the following order:    
Referenced documents  
2  
Terminology  
3  
Significance and use  
4  
Magnification  
5  
Reproduction of photomicrographs  
6  
Optical systems  
7  
Illumination sources  
8  
Illumination of specimens  
9  
Focusing  
10  
Filters for photomicrography  
11  
Illumination techniques  
12  
Instant-processing films  
13  
Photographic materials  
14  
Photographic exposure  
15  
Photographic processing  
16  
Keywords  
17  
Suggestions for visual use of metallographic microscopes  
Appendix X1  
Guide for metallographic photomacrography  
Appendix X2  
Electronic photography  
Appendix X3  
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. Specific precautionary statements are given in X1.7.  
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
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...
SCOPE
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
4.1 These test methods cover four macroscopic and five microscopic test methods (manual and image analysis) for describing the inclusion content of steel and procedures for expressing test results.  
4.2 Inclusions are characterized by size, shape, concentration, and distribution rather than chemical composition. Although compositions are not identified, Microscopic methods place inclusions into one of several composition-related categories (sulfides, oxides, and silicates—the last as a type of oxide). Paragraph 11.1.1 describes a metallographic technique to facilitate inclusion discrimination. Only those inclusions present at the test surface can be detected.  
4.3 The macroscopic test methods evaluate larger surface areas than microscopic test methods and because examination is visual or at low magnifications, these methods are best suited for detecting larger inclusions. Macroscopic methods are not suitable for detecting inclusions smaller than about 0.40 mm (1/64 in.) in length and the methods do not discriminate inclusions by type.  
4.4 The microscopic test methods are employed to characterize inclusions that form as a result of deoxidation or due to limited solubility in solid steel (indigenous inclusions). As stated in 1.1, these microscopic test methods rate inclusion severities and types based on morphological type, that is, by size, shape, concentration, and distribution, but not specifically by composition. These inclusions are characterized by morphological type, that is, by size, shape, concentration, and distribution, but not specifically by composition. The microscopic methods are not intended for assessing the content of exogenous inclusions (those from entrapped slag or refractories). In case of a dispute whether an inclusion is indigenous or exogenous, microanalytical techniques such as energy dispersive X-ray spectroscopy (EDS) may be used to aid in determining the nature of the inclusion. However, experience and knowledge of the casting proce...
SCOPE
1.1 These test methods cover a number of recognized procedures for determining the nonmetallic inclusion content of wrought steel. Macroscopic methods include macroetch, fracture, step-down, and magnetic particle tests. Microscopic methods include five generally accepted systems of examination. In these microscopic methods, inclusions are assigned to a category based on similarities in morphology, and not necessarily on their chemical identity. Metallographic techniques that allow simple differentiation between morphologically similar inclusions are briefly discussed. While the methods are primarily intended for rating inclusions, constituents such as carbides, nitrides, carbonitrides, borides, and intermetallic phases may be rated using some of the microscopic methods. In some cases, alloys other than steels may be rated using one or more of these methods; the methods will be described in terms of their use on steels.  
1.2 These test methods cover procedures to perform JK-type inclusion ratings using automatic image analysis in accordance with microscopic methods A and D.  
1.3 Depending on the type of steel and the properties required, either a macroscopic or a microscopic method for determining the inclusion content, or combinations of the two methods, may be found most satisfactory.  
1.4 These test methods deal only with recommended test methods and nothing in them should be construed as defining or establishing limits of acceptability for any grade of steel.  
1.5 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard.  
1.6 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...

SIGNIFICANCE AND USE
5.1 This test method is established to cover automated SEM/EDX-based procedures for:  
5.1.1 Rating the inclusion content of steels based on procedures listed in Standards E45 and E1245, with the significant difference that the composition of the individual inclusions, as determined by X-ray analysis, is utilized to sort them into chemical classes.  
5.1.2 Determining the number, size and morphological distribution of inclusions in steels sorted by chemical class.  
5.2 Methods 1 and 2 of this test method are primarily intended for rating the inclusion content of steels deoxidized with silicon or aluminum, both silicon and aluminum, or vacuum-treated steels without either silicon or aluminum additions. Guidelines are provided to rate inclusions in steel treated with rare earth additions or calcium-bearing compounds (13.4). When such steels are evaluated, the test report should describe the nature of the inclusions rated according to each inclusion category (A, B, C, D).  
5.3 Methods 1 and 2 will provide a quantitative rating of the inclusion content in half-severity number increments from 0 to 5 for each inclusion type and thickness (Method D of Test Method E45), and in tabulated in Table 2. Test Method E45 ratings by SEM may differ from those determined following E45 because of the use of chemistry in the classifications. In order to differentiate E45 ratings obtained using the SEM from traditional ratings using light microscopy, the ratings obtained using Method 1 or 2 of this Test Method shall be identified as E45-SEM1 and E45-SEM2, respectively.  
5.4 Method 3 defines procedures to analyze and report inclusions by arbitrary size distribution and chemical classifications. It may be made applicable to any material by appropriate choice of these classifications.  
5.4.1 Method 3 determines and reports basic (as used in Test Method E1245) stereological measurements (for example, volume fraction of sulfides and oxides, the number of sulfides or oxides per sq...
SCOPE
1.1 This test method covers procedures to obtain particle size distribution, chemical classification, and Test Methods E45 ratings of inclusions in steels using an automated scanning electron microscope (SEM) with X-ray analysis and automatic image analysis capabilities.  
1.2 There are three discrete methods described. Method 1 is the SEM analog of Test Method E45, which uses image analysis and light microscopy to produce automated Test Methods E45 ratings. Method 2 produces similar ratings based predominantly on sorting inclusions by chemistry into the traditional classes defined in Test Methods E45. Method 3 is recommended when explicit detail is needed on particular inclusion types, not necessarily defined in Test Methods E45, such as to verify the composition of inclusions in inclusion-engineered steel. Method 3 reports stereological parameters such as volume or number fraction, rather than Test Methods E45 type ratings.  
1.3 This test method deals only with the recommended test methods and nothing in it should be construed as defining or establishing limits of acceptability for any grade of steel or other alloy where the method is appropriate.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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
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.
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, 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
5.1 Duplex grain size may occur in some metals and alloys as a result of their thermomechanical processing history. For comparison of mechanical properties with metallurgical features, or for specification purposes, it may be important to be able to characterize grain size in such materials. Assigning an average grain size value to a duplex grain size specimen does not adequately characterize the appearance of that specimen, and may even misrepresent its appearance. For example, averaging two distinctly different grain sizes may result in reporting a size that does not actually exist anywhere in the specimen.  
5.2 These test methods may be applied to specimens or products containing randomly intermingled grains of two or more significantly different sizes (henceforth referred to as random duplex grain size). Examples of random duplex grain sizes include: isolated coarse grains in a matrix of much finer grains, extremely wide distributions of grain sizes, and bimodal distributions of grain size.  
5.3 These test methods may also be applied to specimens or products containing grains of two or more significantly different sizes, but distributed in topologically varying patterns (henceforth referred to as topological duplex grain sizes). Examples of topological duplex grain sizes include: systematic variation of grain size across the section of a product, necklace structures, banded structures, and germinative grain growth in selected areas of critical strain.  
5.4 These test methods may be applied to specimens or products regardless of their state of recrystallization.  
5.5 Because these test methods describe deviations from a single, log-normal distribution of grain sizes, and characterize patterns of variation in grain size, the total specimen cross-section must be evaluated.  
5.6 These test methods are limited to duplex grain sizes as identifiable within a single polished and etched metallurgical specimen. If duplex grain size is suspected in a product too ...
SCOPE
1.1 These test methods provide simple guidelines for deciding whether a duplex grain size exists. The test methods separate duplex grain sizes into one of two distinct classes, then into specific types within those classes, and provide systems for grain size characterization of each type.  
1.2 Units—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 may involve hazardous materials, operations, and equipment. 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.  
1.4 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 is used to assess the indigenous inclusions or second-phase constituents of metals using basic stereological procedures performed by automatic image analyzers.  
5.2 This practice is not suitable for assessing the exogenous inclusions in steels and other metals. Because of the sporadic, unpredictable nature of the distribution of exogenous inclusions, other methods involving complete inspection, for example, ultrasonics, must be used to locate their presence. The exact nature of the exogenous material can then be determined by sectioning into the suspect region followed by serial, step-wise grinding to expose the exogenous matter for identification and individual measurement. Direct size measurement rather than application of stereological methods is employed.  
5.3 Because the characteristics of the indigenous inclusion population vary within a given lot of material due to the influence of compositional fluctuations, solidification conditions and processing, the lot must be sampled statistically to assess its inclusion content. The largest lot sampled is the heat lot but smaller lots, for example, the product of an ingot, within the heat may be sampled as a separate lot. The sampling of a given lot must be adequate for the lot size and characteristics.  
5.4 The practice is suitable for assessment of the indigenous inclusions in any steel (or other metal) product regardless of its size or shape as long as enough different fields can be measured to obtain reasonable statistical confidence in the data. Because the specifics of the manufacture of the product do influence the morphological characteristics of the inclusions, the report should state the relevant manufacturing details, that is, data regarding the deformation history of the product.  
5.5 To compare the inclusion measurement results from different lots of the same or similar types of steels, or other metals, a standard sampling scheme should be adopted such as described in Test Method...
SCOPE
1.1 This practice describes a procedure for obtaining stereological measurements that describe basic characteristics of the morphology of indigenous inclusions in steels and other metals using automatic image analysis. The practice can be applied to provide such data for any discrete second phase.  
Note 1: Stereological measurement methods are used in this practice to assess the average characteristics of inclusions or other second-phase particles on a longitudinal plane-of-polish. This information, by itself, does not produce a three-dimensional description of these constituents in space as deformation processes cause rotation and alignment of these constituents in a preferred manner. Development of such information requires measurements on three orthogonal planes and is beyond the scope of this practice.  
1.2 This practice specifically addresses the problem of producing stereological data when the features of the constituents to be measured make attainment of statistically reliable data difficult.  
1.3 This practice deals only with the recommended test methods and nothing in it should be construed as defining or establishing limits of acceptability.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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
5.1 Qualitative measurement of “nodularity” and “nodule count” using visual estimations has been practiced for many years. These methods suffer from poor reproducibility and repeatability. The introduction of computer-aided image analysis enables metallographers to measure and count individual particles of interest in a microstructure with a high degree of precision. This greatly reduces measurement variations compared to visual estimation methods (see, for example, Test Method A247).  
5.2 This method defines a procedure for measuring the number of nodules and the quality of nodularity of spherulitic graphite in a cast iron microstructure. The specimen’s location in a casting or cast test specimen, and the orientation of the plane-of-polish, are governed by product standards. When a product standard is not defined, choose the test location randomly or at specific systematically chosen depths as needed. The plane-of-polish may be parallel or perpendicular to the solidification direction, or chosen at random, depending upon the needs of the study.  
5.3 This test method may be used to determine variations within a given test specimen, within a given location in a casting, between different locations in a casting, or for the same location in different castings over time. Results from this test method may be used to qualify material for shipment in accordance with guidelines agreed upon between purchaser and manufacturer or can be used to monitor process quality or product variations.  
5.4 Measurements are performed using a computer-controlled automatic image analysis system.  
5.5 A minimum number of specimens and a minimum surface area to be evaluated may be defined by producer-purchaser agreement, provided at least 500 particles meeting the minimum size requirements are measured. The number of particles analyzed shall be indicated in the final analysis report (see 9.6).
SCOPE
1.1 This test method is used to determine the percent nodularity and the nodule count per unit area (that is, number of nodules per mm2) using a light microscopical image of graphite in nodular cast iron. Images generated by other devices, such as a scanning electron microscope, are not specifically addressed, but can be utilized if the system is calibrated in both  x and y directions.  
1.2 Measurement of secondary or temper carbon in other types of cast iron, for example, malleable cast iron or in graphitic tool steels, is not specifically included in this standard because of the different graphite shapes and sizes inherent to such grades  
1.3 This standard deals only with the recommended test method and nothing in it should be construed as defining or establishing limits of acceptability or fitness for purpose of the material tested.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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
5.1 These test methods cover procedures for determining the mean grain size, and the distribution of grain intercept lengths or grain areas, for polycrystalline metals and nonmetallic materials with equiaxed or deformed grain shapes, with uniform or duplex grain size distributions, and for single phase or multiphase grain structures.  
5.2 The measurements are performed using semiautomatic digitizing tablet image analyzers or automatic image analyzers. These devices relieve much of the tedium associated with manual measurements, thus permitting collection of a larger amount of data and more extensive sampling which will produce better statistical definition of the grain size than by manual methods.  
5.3 The precision and relative accuracy of the test results depend on the representativeness of the specimen or specimens, quality of specimen preparation, clarity of the grain boundaries (etch technique and etchant used), the number of grains measured or the measurement area, errors in detecting grain boundaries or grain interiors, errors due to detecting other features (carbides, inclusions, twin boundaries, and so forth), the representativeness of the fields measured, and programming errors.  
5.4 Results from these test methods may be used to qualify material for shipment in accordance with guidelines agreed upon between purchaser and manufacturer, to compare different manufacturing processes or process variations, or to provide data for structure-property-behavior studies.
SCOPE
1.1 These test methods are used to determine grain size from measurements of grain intercept lengths, intercept counts, intersection counts, grain boundary length, and grain areas.  
1.2 These measurements are made with a semiautomatic digitizing tablet or by automatic image analysis using an image of the grain structure produced by a microscope.  
1.3 These test methods are applicable to any type of grain structure or grain size distribution as long as the grain boundaries can be clearly delineated by etching and subsequent image processing, if necessary.  
1.4 These test methods are applicable to measurement of other grain-like microstructures, such as cell structures.  
1.5 This standard deals only with the recommended test methods and nothing in it should be construed as defining or establishing limits of acceptability or fitness for purpose of the materials tested.  
1.6 The sections appear in the following order:    
Section  
Section  
Scope  
1  
Referenced Documents  
2  
Terminology  
3  
Definitions  
3.1  
Definitions of Terms Specific to This Standard  
3.2  
Symbols  
3.3  
Summary of Test Method  
4  
Significance and Use  
5  
Interferences  
6  
Apparatus  
7  
Sampling  
8  
Test Specimens  
9  
Specimen Preparation  
10  
Calibration  
11  
Procedure:  
Semiautomatic Digitizing Tablet  
12  
Intercept Lengths  
12.3  
Intercept and Intersection Counts  
12.4  
Grain Counts  
12.5  
Grain Areas  
12.6  
ALA Grain Size  
12.6.1  
Two-Phase Grain Structures  
12.7  
Procedure:  
Automatic Image Analysis  
13  
Grain Boundary Length  
13.5  
Intersection Counts  
13.6  
Mean Chord (Intercept) Length/Field  
13.7.2  
Individual Chord (Intercept) Lengths  
13.7.4  
Grain Counts  
13.8  
Mean Grain Area/Field  
13.9  
Individual Grain Areas  
13.9.4  
ALA Grain Size  
13.9.8  
Two-Phase Grain Structures  
13.10  
Calculation of Results  
14  
Test Report  
15  
Precision and Bias  
16  
Grain Size of Non-Equiaxed Grain Structure Specimens  
Annex A1  
Examples of Proper and Improper Grain Boundary Delineation  
Annex A2  
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, health, and environmental pra...

SIGNIFICANCE AND USE
2.1 Significance—Retained austenite with a near random crystallographic orientation is found in the microstructure of heat-treated low-alloy, high-strength steels that have medium (0.40 weight %) or higher carbon contents. Although the presence of retained austenite may not be evident in the microstructure, and may not affect the bulk mechanical properties such as hardness of the steel, the transformation of retained austenite to martensite during service can affect the performance of the steel.  
2.2 Use—The measurement of retained austenite can be included in low-alloy steel development programs to determine its effect on mechanical properties. Retained austenite can be measured on a companion specimen or test section that is included in a heat-treated lot of steel as part of a quality control practice. The measurement of retained austenite in steels from service can be included in studies of material performance.
SCOPE
1.1 This test method covers the determination of retained austenite phase in steel using integrated intensities (area under peak above background) of X-ray diffraction peaks using chromium  Kα  or molybdenum Kα  X-radiation.  
1.2 The method applies to carbon and alloy steels with near random crystallographic orientations of both ferrite and austenite phases.  
1.3 This test method is valid for retained austenite contents from 1 % by volume and above.  
1.4 If possible, X-ray diffraction peak interference from other crystalline phases such as carbides should be eliminated from the ferrite and austenite peak intensities.  
1.5 Substantial alloy contents in steel cause some change in peak intensities which have not been considered in this method. Application of this method to steels with total alloy contents exceeding 15 weight % should be done with care. If necessary, the users can calculate the theoretical correction factors to account for changes in volume of the unit cells for austenite and ferrite resulting from variations in chemical composition.  
1.6 Units—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.  
1.7 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.8 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
3.1 Standards of Committee E04 consist of test methods, practices, and guides developed to ensure proper and uniform testing in the field of metallography. In order for one to properly use and interpret these standards, the terminology used in these standards must be understood.  
3.2 The terms used in the field of metallography have precise definitions. The terminology and its proper usage must be completely understood in order to adequately communicate in this field. In this respect, this standard is also a general source of terminology relating to the field of metallography facilitating the transfer of information within the field.

SIGNIFICANCE AND USE
5.1 Hardness tests have been found to be very useful for materials evaluation, quality control of manufacturing processes and research and development efforts. Hardness, although empirical in nature, can be correlated to tensile strength for many metals and alloys, and is also an indicator of machinability, wear resistance, toughness and ductility.  
5.2 Microindentation tests are utilized to evaluate and quantify hardness variations that occur over a small distance. These variations may be intentional, such as produced by localized surface hardening, for example, from shot blasting, cold drawing, flame hardening, induction hardening, etc., or from processes such as carburization, nitriding, carbonitriding, etc.; or, they may be unintentional variations due to problems, such as decarburization, localized softening in service, or from compositional/microstructural segregation problems. Low test forces also extend hardness testing to materials too thin or too small for macroindentation tests. Microindentation tests permit hardness testing of specific phases or constituents and regions or gradients too small for evaluation by macroindentation tests.  
5.3 Because microindentation hardness tests will reveal hardness variations that commonly exist within most materials, a single test value may not be representative of the bulk hardness. Vickers tests at 1000 gf can be utilized for determination of the bulk hardness, but, as for any hardness test, it is recommended that a number of indents are made and the average and standard deviation are calculated, as needed or as required.  
5.4 Microindentation hardness testing is generally performed to quantify variations in hardness that occur over small distances. To determine these differences requires a very small physical indentation. Testers that create indents at very low test forces must be carefully constructed to accurately apply the test forces exactly at the desired location and must have a high-quality optical syste...
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1.1 This test method covers determination of the microindentation hardness of materials.  
1.2 This test method covers microindentation tests made with Knoop and Vickers indenters under test forces in the range from 9.8 × 10-3 to 9.8 N (1 to 1000 gf).  
1.3 This test method includes an analysis of the possible sources of errors that can occur during microindentation testing and how these factors affect the precision, bias, repeatability, and reproducibility of test results.  
1.4 Information pertaining to the requirements for direct verification and calibration of the testing machine and the requirements for the manufacture and calibration of Vickers and Knoop reference hardness test blocks are in Test Method E92.
Note 1: While Committee E04 is primarily concerned with metals, the test procedures described are applicable to other materials.  
1.5 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 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.  
1.7 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 These test methods cover procedures for estimating and rules for expressing the average grain size of all metals consisting entirely, or principally, of a single phase. The grain size of specimens with two phases, or a phase and a constituent, can be measured using a combination of two methods, a measurement of the volume fraction of the phase and an intercept or planimetric count (see Section 17). The test methods may also be used for any structures having appearances similar to those of the metallic structures shown in the comparison charts. The three basic procedures for grain size estimation are:  
4.1.1 Comparison Procedure—The comparison procedure does not require counting of either grains, intercepts, or intersections but, as the name suggests, involves comparison of the grain structure to a series of graded images, either in the form of a wall chart, clear plastic overlays, or an eyepiece reticle. There appears to be a general bias in that comparison grain size ratings claim that the grain size is somewhat coarser (1/2 to 1 G number lower) than it actually is (see X1.3.5). Repeatability and reproducibility of comparison chart ratings are generally ±1 grain size number.  
4.1.2 Planimetric Procedure—The planimetric method involves an actual count of the number of grains within a known area. The number of grains per unit area, NA , is used to determine the ASTM grain size number, G. The precision of the method is a function of the number of grains counted. A precision of ±0.25 grain size units can be attained with a reasonable amount of effort. Results are free of bias and repeatability and reproducibility are less than ±0.5 grain size units. An accurate count does require marking off of the grains as they are counted.  
4.1.3 Intercept Procedure—The intercept method involves an actual count of the number of grains intercepted by a test line or the number of grain boundary intersections with a test line, per unit length of test line, used to calculate t...
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1.1 These test methods cover the measurement of average grain size and include the comparison procedure, the planimetric (or Jeffries) procedure, and the intercept procedures. These test methods may also be applied to nonmetallic materials with structures having appearances similar to those of the metallic structures shown in the comparison charts. These test methods apply chiefly to single phase grain structures but they can be applied to determine the average size of a particular type of grain structure in a multiphase or multiconstituent specimen.  
1.2 These test methods are used to determine the average grain size of specimens with a unimodal distribution of grain areas, diameters, or intercept lengths. These distributions are approximately log normal. These test methods do not cover methods to characterize the nature of these distributions. Characterization of grain size in specimens with duplex grain size distributions is described in Test Methods E1181. Measurement of individual, very coarse grains in a fine grained matrix is described in Test Methods E930.  
1.3 These test methods deal only with determination of planar grain size, that is, characterization of the two-dimensional grain sections revealed by the sectioning plane. Determination of spatial grain size, that is, measurement of the size of the three-dimensional grains in the specimen volume, is beyond the scope of these test methods.  
1.4 These test methods describe techniques performed manually using either a standard series of graded chart images for the comparison method or simple templates for the manual counting methods. Utilization of semi-automatic digitizing tablets or automatic image analyzers to measure grain size is described in Test Methods E1382.  
1.5 These test methods deal only with the recommended test methods and nothing in them should be construed as defining or establishing limits of acceptability or fitness of purpose of the ma...

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
4.1 TSCs are susceptible to the formation of porosity due to a lack of fusion between sprayed particles or the expansion of gases generated during the spraying process. The determination of area percent porosity is important in order to monitor the effect of variable spray parameters and the suitability of a coating for its intended purpose. Depending on application, some or none of this porosity may be tolerable.  
4.2 These test methods cover the determination of the area percentage porosity of TSCs. Method A is a manual, direct comparison method utilizing the seven standard images in Figs. 1-7 which depict typical distributions of porosity in TSCs. Method B is an automated technique requiring the use of a computerized image analyzer.
FIG. 1 — 0.5 % Porosity  
FIG. 2 — 1.0 % Porosity  
FIG. 3 — 2.0 % Porosity  
FIG. 4 — 5.0 % Porosity  
FIG. 5 — 8.0 % Porosity  
FIG. 6 — 10.0 % Porosity  
FIG. 7 — 15.0 % Porosity  
4.3 These methods quantify area percent porosity only on the basis of light reflectivity from a metallographically polished cross section. See Guide E1920 for recommended metallographic preparation procedures.  
4.4 The person using these test methods must be familiar with the visual features of TSCs and be able to determine differences between inherent porosity and oxides. The individual must be aware of the possible types of artifacts that may be created during sectioning and specimen preparation, for example, pullouts and smearing, so that results are reported only on properly prepared specimens. Examples of properly prepared specimens are shown in Figs. 8-10. If there are doubts as to the integrity of the specimen preparation it is suggested that other means be used to confirm microstructural features. This may include energy dispersive spectroscopy (EDS), wavelength dispersive spectroscopy (WDS) or cryogenic fracture of the coating followed by analysis of the fractured surfaces with a scanning electron microscope (SEM).
FIG. 8 Ni/Al T...
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1.1 These test methods cover procedures to perform porosity ratings on metallographic specimens of thermal sprayed coatings (TSCs) prepared in accordance with Guide E1920 by direct comparison to standard images and via the use of automatic image analysis equipment.  
1.2 These test methods deal only with recommended measuring methods and nothing in them should be construed as defining or establishing limits of acceptability for any measured value of porosity.  
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.  
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 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 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
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
5.1 These test methods are used to detect surface losses in carbon content due to heating at elevated temperatures, as in hot working or heat treatment.  
5.2 Results of such tests may be used to qualify material for shipment according to agreed upon guidelines between purchaser and manufacturer, for guidance as to machining allowances, or to assess the influence of processing upon decarburization tendency.  
5.3 Screening tests are simple, fast, low-cost tests designed to separate non-decarburized samples from those with appreciable decarburization. Based on the results of such tests, the other procedures may be utilized as applicable.  
5.4 Microscopical tests require a metallographically polished cross section to permit reasonably accurate determination of the depth and nature of the decarburization present. Several methods may be employed for estimation of the depth of decarburization. The statistical accuracy of each varies with the amount of effort expended.  
5.5 Microindentation hardness methods are employed on polished cross sections and are most suitable for hardened specimens with reasonably uniform microstructures. This procedure can be used to define the depth to a specific minimum hardness or the depth to a uniform hardness.  
5.6 Chemical analytical methods are limited to specimens with simple, uniform shapes and are based on analysis of incremental turnings or after milling at fixed increments.  
5.7 Microscopical tests are generally satisfactory for determining the suitability of material for intended use, specification acceptance, manufacturing control, development, or research.
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1.1 These test methods cover procedures for estimating the depth of decarburization of steels irrespective of the composition, matrix microstructure, or section shape. The following basic procedures may be used:  
1.1.1 Screening methods.  
1.1.2 Microscopical methods.  
1.1.3 Microindentation hardness methods.  
1.1.4 Chemical analysis methods.  
1.2 In case of a dispute, the rigorous quantitative or lineal analysis method (see 7.3.5 and 7.3.6) shall be the referee method. These methods can be employed with any cross-sectional shape. The chemical analytical methods generally reveal a greater depth of decarburization than the microscopical methods but are limited to certain simple shapes and by availability of equipment. These techniques are generally reserved for research studies. The microindentation hardness method is suitable for accurate measurements of hardened structures with relatively homogeneous microstructures.  
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 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 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
5.1 This guide covers procedures for quantifying the elemental composition of phases in a microstructure. It includes both methods that use standards as well as standardless methods, and it discusses the precision and accuracy that one can expect from the technique. The guide applies to EDS with a solid-state X-ray detector used on an SEM or EPMA.  
5.2 EDS is a suitable technique for routine quantitative analysis of elements that are 1) heavier than or equal to sodium in atomic weight, 2) present in tenths of a percent or greater by weight, and 3) occupying a few cubic micrometres, or more, of the specimen. Elements of lower atomic number than sodium can be analyzed with either ultra-thin-window or windowless spectrometers, generally with less precision than is possible for heavier elements. Trace elements, defined as 2 can be analyzed but with lower precision compared with analyses of elements present in greater concentration.
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1.1 This guide is intended to assist those using energy-dispersive spectroscopy (EDS) for quantitative analysis of materials with a scanning electron microscope (SEM) or electron probe microanalyzer (EPMA). It is not intended to substitute for a formal course of instruction, but rather to provide a guide to the capabilities and limitations of the technique and to its use. For a more detailed treatment of the subject, see Goldstein, et al. (1) This guide does not cover EDS with a transmission electron microscope (TEM).  
1.2 Units—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.  
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 Proper use of this practice can yield calibrated magnifications with precision of 5 % or better within a magnification range of from 10 to 50 000X.  
4.2 The use of calibration specimens traceable to international/national standards, such as NIST-SRM 484, with this practice will yield magnifications accurate to better than 5 % over the calibrated range of operating conditions.  
4.3 The accuracy of the calibrated magnifications, or dimensional measurements, will be poorer than the accuracy of the calibration specimen used with this practice.  
4.4 For accuracy approaching that of the calibration specimen this practice must be applied with the identical operating conditions (accelerating voltage, working distance and magnification) used to image the specimens of interest.  
4.5 It is incumbent upon each facility using this practice to define the standard range of magnification and operating conditions as well as the desired accuracy for which this practice will be applied. The standard operating conditions must include those parameters which the operator can control including: accelerating voltage, working distance, magnification, and imaging mode.
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1.1 This practice covers general procedures necessary for the calibration of magnification of scanning electron microscopes. The relationship between true magnification and indicated magnification is a complicated function of operating conditions.2 Therefore, this practice must be applied to each set of standard operating conditions to be used.  
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.  
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 These methods can be used to determine magnifications as viewed through the eyepieces of light microscopes.  
4.2 These methods can be used to calibrate microscope magnifications for photography, video systems, and projection stations.  
4.3 Reticles may be calibrated as independent articles and as components of a microscope system.
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1.1 This guide covers methods for calculating and calibrating microscope magnifications, photographic magnifications, video monitor magnifications, grain size comparison reticles, and other measuring reticles. Reflected light microscopes are used to characterize material microstructures. Many materials engineering decisions may be based on qualitative and quantitative analyses of a microstructure. It is essential that microscope magnifications and reticle dimensions be accurate.  
1.2 The calibration using these methods is only as precise as the measuring devices used. It is recommended that the stage micrometer or scale used in the calibration should be traceable to the National Institute of Standards and Technology (NIST) or a similar organization.  
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.  
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 provides a way to estimate the average grain size of polycrystalline materials. It is based on EBSD measurements of crystallographic orientation which are inherently quantitative in nature. This method has specific advantage over traditional optical grain size measurements in some materials, where it is difficult to find appropriate metallographic preparation procedures to adequately delineate grain boundaries.
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1.1 This practice is used to determine grain size from measurements of grain areas from automated electron backscatter diffraction (EBSD) scans of polycrystalline materials.  
1.2 The intent of this practice is to standardize operation of an automated EBSD instrument to measure ASTM G directly from crystal orientation. The guidelines and caveats of E112 apply here, but the focus of this standard is on EBSD practice.  
1.3 This practice is only applicable to fully recrystallized materials.  
1.4 This practice is applicable to any crystalline material which produces EBSD patterns of sufficient quality that a high percentage of the patterns can be reliably indexed using automated indexing software.  
1.5 The practice is applicable to any type of grain structure or grain size distribution.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.8 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.

ABSTRACT
This practice describes a methodology to statistically characterize the distribution of the largest indigenous non-metallic inclusions in steel specimens based upon quantitative metallographic measurements. This practice enables the experimenter to estimate the extreme value distribution of inclusions in steels. The procedures in determining non-metallic inclusions in steel are presented and discussed in details.
SIGNIFICANCE AND USE
5.1 This practice is used to assess the indigenous inclusions or second-phase constituents in metals using extreme value statistics.  
5.2 It is well known that failures of mechanical components, such as gears and bearings, are often caused by the presence of large nonmetallic oxide inclusions. Failure of a component can often be traced to the presence of a large inclusion. Predictions related to component fatigue life are not possible with the evaluations provided by standards such as Test Methods E45, Practice E1122, or Practice E1245. The use of extreme value statistics has been related to component life and inclusion size distributions by several different investigators (3-8). The purpose of this practice is to create a standardized method of performing this analysis.  
5.3 This practice is not suitable for assessing the exogenous inclusions in steels and other metals because of the unpredictable nature of the distribution of exogenous inclusions. Other methods involving complete inspection such as ultrasonics must be used to locate their presence.
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1.1 This practice describes a methodology to statistically characterize the distribution of the largest indigenous nonmetallic inclusions in steel specimens based upon quantitative metallographic measurements. The practice is not suitable for assessing exogenous inclusions.  
1.2 Based upon the statistical analysis, the nonmetallic content of different lots of steels can be compared.  
1.3 This practice deals only with the recommended test methods and nothing in it should be construed as defining or establishing limits of acceptability.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4.1 For measurements obtained from light microscopy, linear feature parameters shall be reported as micrometers, and feature areas shall be reported as micrometers.  
1.5 The methodology can be extended to other materials and to other microstructural features.  
1.6 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.  
1.7 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 The physical properties of metals and other materials are often anisotropic (for example: Young's modulus will typically vary in different crystallographic directions). As such, it is often desirable or necessary to determine the orientation of a single crystal to ascertain the relation of any pertinent physical properties with respect to different directions in the material.  
4.2 This test method can be used commercially as a quality control test in production situations in which a desired orientation, within prescribed limits, is required.  
4.3 With the use of an adjustable, fixed holder that can later be mounted on a saw, lathe, or other machine, a single crystal material can be moved to a preferred orientation and subsequently sectioned, ground, or processed otherwise.  
4.4 If the grains in a polycrystalline material are large enough, this test method can also be used to determine their orientations and differences in orientation can be documented or mapped or both.
SCOPE
1.1 This test method covers the back-reflection Laue procedure for determining the orientation of a metal crystal. The back-reflection Laue method for determining crystal orientation may be applied to macrograins and micrograins depending on the beam size within polycrystalline aggregates, as well as to single crystals of any size. This test method is described with reference to cubic crystals and other structures such as: hexagonal, tetragonal, or orthorhombic crystals.  
1.2 Most natural crystals have well developed external faces, and the orientation of such crystals can usually be determined from inspection. The orientation of a crystal having poorly developed faces or no faces at all (for example, a metal crystal prepared in the laboratory) shall be determined by more elaborate methods. The most convenient and accurate of these involves the use of X-ray diffraction. The “orientation of a metal crystal” is known when the positions in space of the crystallographic axes of the unit cell have been located with reference to the surface geometry of the crystal specimen. This relation between unit cell position and surface geometry is most conveniently expressed by stereographic or gnomonic projection.  
1.3 Units—The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in non-conformance with the standard.  
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
5.1 This test method is based upon the stereological principle that a grid with a number of regularly arrayed points, when systematically placed over an image of a two-dimensional section through the microstructure, can provide, after a representative number of placements on different fields, an unbiased statistical estimation of the volume fraction of an identifiable constituent or phase (1, 2, 3).3  
5.2 This test method has been described  (4) as being superior to other manual methods with regard to effort, bias, and simplicity.  
5.3 Any number of clearly distinguishable constituents or phases within a microstructure (or macrostructure) can be counted using the method. Thus, the method can be applied to any type of solid material from which adequate two-dimensional sections can be prepared and observed.  
5.4 A condensed step-by-step guide for using the method is given in Annex A1.
SCOPE
1.1 This test method describes a systematic manual point counting procedure for statistically estimating the volume fraction of an identifiable constituent or phase from sections through the microstructure by means of a point grid.  
1.2 The use of automatic image analysis to determine the volume fraction of constituents is described in Practice E1245.  
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 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
5.1 This practice is used to assess the nature and extent of banding or orientation of microstructures of metals and other materials where deformation and processing produce a banded or oriented condition.  
5.2 Banded or oriented microstructures can arise in single phase, two phase or multiphase metals and materials. The appearance of the orientation or banding is influenced by processing factors such as the solidification rate, the extent of segregation, the degree of hot or cold working, the nature of the deformation process used, the heat treatments, and so forth.  
5.3 Microstructural banding or orientation influence the uniformity of mechanical properties determined in various test directions with respect to the deformation direction.  
5.4 The stereological methods can be applied to measure the nature and extent of microstructural banding or orientation for any metal or material. The microindentation hardness test procedure should only be used to determine the difference in hardness in banded heat-treated metals, chiefly steels.  
5.5 Isolated segregation may also be present in an otherwise reasonably homogeneous microstructure. Stereological methods are not suitable for measuring individual features, instead use standard measurement procedures to define the feature size. The microindentation hardness method may be used for such structures.  
5.6 Results from these test methods may be used to qualify material for shipment in accordance with guidelines agreed upon between purchaser and manufacturer, for comparison of different manufacturing processes or process variations, or to provide data for structure-property-behavior studies.
SCOPE
1.1 This practice describes a procedure to qualitatively describe the nature of banded or oriented microstructures based on the morphological appearance of the microstructure.  
1.2 This practice describes stereological procedures for quantitative measurement of the degree of microstructural banding or orientation.  
Note 1: Although stereological measurement methods are used to assess the degree of banding or alignment, the measurements are only made on planes parallel to the deformation direction (that is, a longitudinal plane) and the three-dimensional characteristics of the banding or alignment are not evaluated.  
1.3 This practice describes a microindentation hardness test procedure for assessing the magnitude of the hardness differences present in banded heat-treated steels. For fully martensitic carbon and alloy steels (0.10–0.65 %C), in the as-quenched condition, the carbon content of the matrix and segregate may be estimated from the microindentation hardness values.  
1.4 This practice does not cover chemical analytical methods for evaluating banded structures.  
1.5 This practice deals only with the recommended test methods and nothing in it should be construed as defining or establishing limits of acceptability.  
1.6 The measured values are stated in SI units, which are regarded as standard. Equivalent inch-pound values, when listed, are in parentheses and may be approximate.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.8 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 The presence of large grains has been correlated with anomalous mechanical behavior in, for example, crack initiation, crack propagation, and fatigue. Thus there is engineering justification for reporting the ALA grain size.  
4.2 These methods shall only be used with the presence of outlier coarse grains, 3 or more ASTM grain size numbers larger than the rest of the microstructure and comprising 5 % or less of the specimen area. A typical example is shown in Annex A1 as Fig. A1.1.  
4.3 These methods shall not be used for the determination of average grain size, which is treated in Test Methods E112. Examples of microstructures that do not qualify for ALA treatment are shown in Annex A1 as Fig. A1.2, Fig. A1.3, and Fig. A1.4.  
4.4 These methods may be applied in the characterization of duplex grain sizes, as instructed in the procedures for Test Methods E1181.
SCOPE
1.1 These test methods describe simple manual procedures for measuring the size of the largest grain cross-section observed on a metallographically prepared plane section.  
1.2 These test methods shall only be valid for microstructures containing outlier coarse grains, where their population is too sparse for grain size determination by Test Methods E112.  
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.  
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 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.  
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.
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.  
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 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.
SCOPE
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
5.1 This test method is based upon the stereological principle that a grid with a number of regularly arrayed points, when systematically placed over an image of a two-dimensional section through the microstructure, can provide, after a representative number of placements on different fields, an unbiased statistical estimation of the volume fraction of an identifiable constituent or phase (1, 2, 3).3  
5.2 This test method has been described  (4) as being superior to other manual methods with regard to effort, bias, and simplicity.  
5.3 Any number of clearly distinguishable constituents or phases within a microstructure (or macrostructure) can be counted using the method. Thus, the method can be applied to any type of solid material from which adequate two-dimensional sections can be prepared and observed.  
5.4 A condensed step-by-step guide for using the method is given in Annex A1.
SCOPE
1.1 This test method describes a systematic manual point counting procedure for statistically estimating the volume fraction of an identifiable constituent or phase from sections through the microstructure by means of a point grid.  
1.2 The use of automatic image analysis to determine the volume fraction of constituents is described in Practice E1245.  
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 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 These test methods cover four macroscopic and five microscopic test methods (manual and image analysis) for describing the inclusion content of steel and procedures for expressing test results.  
4.2 Inclusions are characterized by size, shape, concentration, and distribution rather than chemical composition. Although compositions are not identified, Microscopic methods place inclusions into one of several composition-related categories (sulfides, oxides, and silicates—the last as a type of oxide). Paragraph 11.1.1 describes a metallographic technique to facilitate inclusion discrimination. Only those inclusions present at the test surface can be detected.  
4.3 The macroscopic test methods evaluate larger surface areas than microscopic test methods and because examination is visual or at low magnifications, these methods are best suited for detecting larger inclusions. Macroscopic methods are not suitable for detecting inclusions smaller than about 0.40 mm (1/64 in.) in length and the methods do not discriminate inclusions by type.  
4.4 The microscopic test methods are employed to characterize inclusions that form as a result of deoxidation or due to limited solubility in solid steel (indigenous inclusions). As stated in 1.1, these microscopic test methods rate inclusion severities and types based on morphological type, that is, by size, shape, concentration, and distribution, but not specifically by composition. These inclusions are characterized by morphological type, that is, by size, shape, concentration, and distribution, but not specifically by composition. The microscopic methods are not intended for assessing the content of exogenous inclusions (those from entrapped slag or refractories). In case of a dispute whether an inclusion is indigenous or exogenous, microanalytical techniques such as energy dispersive X-ray spectroscopy (EDS) may be used to aid in determining the nature of the inclusion. However, experience and knowledge of the casting proce...
SCOPE
1.1 These test methods cover a number of recognized procedures for determining the nonmetallic inclusion content of wrought steel. Macroscopic methods include macroetch, fracture, step-down, and magnetic particle tests. Microscopic methods include five generally accepted systems of examination. In these microscopic methods, inclusions are assigned to a category based on similarities in morphology, and not necessarily on their chemical identity. Metallographic techniques that allow simple differentiation between morphologically similar inclusions are briefly discussed. While the methods are primarily intended for rating inclusions, constituents such as carbides, nitrides, carbonitrides, borides, and intermetallic phases may be rated using some of the microscopic methods. In some cases, alloys other than steels may be rated using one or more of these methods; the methods will be described in terms of their use on steels.  
1.2 These test methods cover procedures to perform JK-type inclusion ratings using automatic image analysis in accordance with microscopic methods A and D.  
1.3 Depending on the type of steel and the properties required, either a macroscopic or a microscopic method for determining the inclusion content, or combinations of the two methods, may be found most satisfactory.  
1.4 These test methods deal only with recommended test methods and nothing in them should be construed as defining or establishing limits of acceptability for any grade of steel.  
1.5 The values stated in SI units are to be regarded as the standard. Values in parentheses are conversions and are approximate.  
1.6 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.  
1.7 This internationa...

SIGNIFICANCE AND USE
5.1 This practice is used to assess the nature and extent of banding or orientation of microstructures of metals and other materials where deformation and processing produce a banded or oriented condition.  
5.2 Banded or oriented microstructures can arise in single phase, two phase or multiphase metals and materials. The appearance of the orientation or banding is influenced by processing factors such as the solidification rate, the extent of segregation, the degree of hot or cold working, the nature of the deformation process used, the heat treatments, and so forth.  
5.3 Microstructural banding or orientation influence the uniformity of mechanical properties determined in various test directions with respect to the deformation direction.  
5.4 The stereological methods can be applied to measure the nature and extent of microstructural banding or orientation for any metal or material. The microindentation hardness test procedure should only be used to determine the difference in hardness in banded heat-treated metals, chiefly steels.  
5.5 Isolated segregation may also be present in an otherwise reasonably homogeneous microstructure. Stereological methods are not suitable for measuring individual features, instead use standard measurement procedures to define the feature size. The microindentation hardness method may be used for such structures.  
5.6 Results from these test methods may be used to qualify material for shipment in accordance with guidelines agreed upon between purchaser and manufacturer, for comparison of different manufacturing processes or process variations, or to provide data for structure-property-behavior studies.
SCOPE
1.1 This practice describes a procedure to qualitatively describe the nature of banded or oriented microstructures based on the morphological appearance of the microstructure.  
1.2 This practice describes stereological procedures for quantitative measurement of the degree of microstructural banding or orientation.  
Note 1: Although stereological measurement methods are used to assess the degree of banding or alignment, the measurements are only made on planes parallel to the deformation direction (that is, a longitudinal plane) and the three-dimensional characteristics of the banding or alignment are not evaluated.  
1.3 This practice describes a microindentation hardness test procedure for assessing the magnitude of the hardness differences present in banded heat-treated steels. For fully martensitic carbon and alloy steels (0.10–0.65 %C), in the as-quenched condition, the carbon content of the matrix and segregate may be estimated from the microindentation hardness values.  
1.4 This standard does not cover chemical analytical methods for evaluating banded structures.  
1.5 This practice deals only with the recommended test methods and nothing in it should be construed as defining or establishing limits of acceptability.  
1.6 The measured values are stated in SI units, which are regarded as standard. Equivalent inch-pound values, when listed, are in parentheses and may be approximate.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.8 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 These test methods cover four macroscopic and five microscopic test methods (manual and image analysis) for describing the inclusion content of steel and procedures for expressing test results.  
4.2 Inclusions are characterized by size, shape, concentration, and distribution rather than chemical composition. Although compositions are not identified, Microscopic methods place inclusions into one of several composition-related categories (sulfides, oxides, and silicates—the last as a type of oxide). Paragraph 12.2.1 describes a metallographic technique to facilitate inclusion discrimination. Only those inclusions present at the test surface can be detected.  
4.3 The macroscopic test methods evaluate larger surface areas than microscopic test methods and because examination is visual or at low magnifications, these methods are best suited for detecting larger inclusions. Macroscopic methods are not suitable for detecting inclusions smaller than about 0.40 mm (1/64 in.) in length and the methods do not discriminate inclusions by type.  
4.4 The microscopic test methods are employed to characterize inclusions that form as a result of deoxidation or due to limited solubility in solid steel (indigenous inclusions). As stated in 1.1, these microscopic test methods rate inclusion severities and types based on morphological type, that is, by size, shape, concentration, and distribution, but not specifically by composition. These inclusions are characterized by morphological type, that is, by size, shape, concentration, and distribution, but not specifically by composition. The microscopic methods are not intended for assessing the content of exogenous inclusions (those from entrapped slag or refractories). In case of a dispute whether an inclusion is indigenous or exogenous, microanalytical techniques such as energy dispersive X-ray spectroscopy (EDS) may be used to aid in determining the nature of the inclusion. However, experience and knowledge of the casting proce...
SCOPE
1.1 These test methods cover a number of recognized procedures for determining the nonmetallic inclusion content of wrought steel. Macroscopic methods include macroetch, fracture, step-down, and magnetic particle tests. Microscopic methods include five generally accepted systems of examination. In these microscopic methods, inclusions are assigned to a category based on similarities in morphology, and not necessarily on their chemical identity. Metallographic techniques that allow simple differentiation between morphologically similar inclusions are briefly discussed. While the methods are primarily intended for rating inclusions, constituents such as carbides, nitrides, carbonitrides, borides, and intermetallic phases may be rated using some of the microscopic methods. In some cases, alloys other than steels may be rated using one or more of these methods; the methods will be described in terms of their use on steels.  
1.2 These test methods cover procedures to perform JK-type inclusion ratings using automatic image analysis in accordance with microscopic methods A and D.  
1.3 Depending on the type of steel and the properties required, either a macroscopic or a microscopic method for determining the inclusion content, or combinations of the two methods, may be found most satisfactory.  
1.4 These test methods deal only with recommended test methods and nothing in them should be construed as defining or establishing limits of acceptability for any grade of steel.  
1.5 The values stated in SI units are to be regarded as the standard. Values in parentheses are conversions and are approximate.  
1.6 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.  
1.7 This internationa...

SIGNIFICANCE AND USE
3.1 Standards of Committee E04 consist of test methods, practices, and guides developed to ensure proper and uniform testing in the field of metallography. In order for one to properly use and interpret these standards, the terminology used in these standards must be understood.  
3.2 The terms used in the field of metallography have precise definitions. The terminology and its proper usage must be completely understood in order to adequately communicate in this field. In this respect, this standard is also a general source of terminology relating to the field of metallography facilitating the transfer of information within the field.

SIGNIFICANCE AND USE
5.1 Hardness tests have been found to be very useful for materials evaluation, quality control of manufacturing processes and research and development efforts. Hardness, although empirical in nature, can be correlated to tensile strength for many metals and alloys, and is also an indicator of machinability, wear resistance, toughness and ductility.  
5.2 Microindentation tests are utilized to evaluate and quantify hardness variations that occur over a small distance. These variations may be intentional, such as produced by localized surface hardening, for example, from shot blasting, cold drawing, flame hardening, induction hardening, etc., or from processes such as carburization, nitriding, carbonitriding, etc.; or, they may be unintentional variations due to problems, such as decarburization, localized softening in service, or from compositional/microstructural segregation problems. Low test forces also extend hardness testing to materials too thin or too small for macroindentation tests. Microindentation tests permit hardness testing of specific phases or constituents and regions or gradients too small for evaluation by macroindentation tests.  
5.3 Because microindentation hardness tests will reveal hardness variations that commonly exist within most materials, a single test value may not be representative of the bulk hardness. Vickers tests at 1000 gf can be utilized for determination of the bulk hardness, but, as for any hardness test, it is recommended that a number of indents are made and the average and standard deviation are calculated, as needed or as required.  
5.4 Microindentation hardness testing is generally performed to quantify variations in hardness that occur over small distances. To determine these differences requires a very small physical indentation. Testers that create indents at very low test forces must be carefully constructed to accurately apply the test forces exactly at the desired location and must have a high-quality optical syste...
SCOPE
1.1 This test method covers determination of the microindentation hardness of materials.  
1.2 This test method covers microindentation tests made with Knoop and Vickers indenters under test forces in the range from 9.8 × 10-3 to 9.8 N (1 to 1000 gf).  
1.3 This test method includes an analysis of the possible sources of errors that can occur during microindentation testing and how these factors affect the precision, bias, repeatability, and reproducibility of test results.  
1.4 Information pertaining to the requirements for direct verification and calibration of the testing machine and the requirements for the manufacture and calibration of Vickers and Knoop reference hardness test blocks are in Test Method E92.
Note 1: While Committee E04 is primarily concerned with metals, the test procedures described are applicable to other materials.  
1.5 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 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.  
1.7 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 The traditional resolution test of the SEM requires, as a first step, a photomicrograph of a fine particulate sample taken at a high magnification. The operator is required to measure a distance on the photomicrograph between two adjacent, but separate edges. These edges are usually less than one millimetre apart. Their image quality is often less than optimum limited by the S/N ratio of a beam with such a small diameter and low current. Operator judgment is dependent on the individual acuity of the person making the measurement and can vary significantly.  
4.2 Use of this practice results in SEM electron beam size characterization which is significantly more reproducible than the traditional resolution test using a fine particulate sample.
SCOPE
1.1 This practice provides a reproducible means by which one aspect of the performance of a scanning electron microscope (SEM) may be characterized. The resolution of an SEM depends on many factors, some of which are electron beam voltage and current, lens aberrations, contrast in the specimen, and operator-instrument-material interaction. However, the resolution for any set of conditions is limited by the size of the electron beam. This size can be quantified through the measurement of an effective apparent edge sharpness for a number of materials, two of which are suggested. This practice requires an SEM with the capability to perform line-scan traces, for example, Y-deflection waveform generation, for the suggested materials. The range of SEM magnification at which this practice is of utility is from 1000 to 50 000 × . Higher magnifications may be attempted, but difficulty in making precise measurements can be expected.  
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
3.1 Pole figures are two-dimensional graphic representations, on polar coordinate paper, of the average distribution of crystallite orientations in three dimensions. Data for constructing pole figures are obtained with X-ray diffractometers, using reflection and transmission techniques.  
3.2 Several alternative procedures may be used. Some produce complete pole figures. Others yield partial pole figures, which may be combined to produce a complete figure.
SCOPE
1.1 This test method covers the use of the X-ray diffractometer to prepare quantitative pole figures.  
1.2 The test method consists of several experimental procedures. Some of the procedures (1-5)2 permit preparation of a complete pole figure. Others must be used in combination to produce a complete pole figure.  
1.3 Pole figures (6)  and inverse pole figures (7-10)  are two dimensional averages of the three-dimensional crystallite orientation distribution. Pole figures may be used to construct either inverse pole figures (11-13)  or the crystallite orientation distribution (14-21). Development of series expansions of the crystallite orientation distribution from reflection pole figures (22, 23)  makes it possible to obtain a series expansion of a complete pole figure from several incomplete pole figures. Pole figures or inverse pole figures derived by such methods shall be termed calculated. These techniques will not be described herein.  
1.4 Provided the orientation is homogeneous through the thickness of the sheet, certain procedures  (1-3)  may be used to obtain a complete pole figure.  
1.5 Provided the orientation has mirror symmetry with respect to planes perpendicular to the rolling, transverse, and normal directions, certain procedures (4, 5, 24)  may be used to obtain a complete pole figure.  
1.6 The test method emphasizes the Schulz reflection technique (25).  Other techniques (3, 4, 5, 24)  may be considered variants of the Schulz technique and are cited as options, but not described herein.  
1.7 The test method also includes a description of the transmission technique of Decker, et al (26),  which may be used in conjunction with the Schulz reflection technique to obtain a complete pole figure.  
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.  
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 This guide is useful for the photomicrography and photomacrography of metals and other materials.  
4.2 The subsequent processing of the photographic materials is also treated.
SCOPE
1.1 This guide outlines various methods which may be followed in the photography of metals and materials with the reflected-light microscope. Methods are included for preparation of prints and transparencies in black-and-white and in color, using both direct rapid and wet processes.  
1.2 Guidelines are suggested to yield photomicrographs of typical subjects and, to the extent possible, of atypical subjects as well. Information is included concerning techniques for the enhanced display of specific material features. Descriptive material is provided where necessary to clarify procedures. References are cited where detailed descriptions may be helpful.  
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 requirements prior to use. Specific precautionary statements are given in X1.7.  
1.4 The sections appear in the following order:    
Referenced documents  
2  
Terminology  
3  
Significance and use  
4  
Magnification  
5  
Reproduction of photomicrographs  
6  
Optical systems  
7  
Illumination sources  
8  
Illumination of specimens  
9  
Focusing  
10  
Filters for photomicrography  
11  
Illumination techniques  
12  
Instant-processing films  
13  
Photographic materials  
14  
Photographic exposure  
15  
Photographic processing  
16  
Keywords  
17  
Suggestions for visual use of metallographic microscopes  
Appendix X1  
Guide for metallographic photomacrography  
Appendix X2  
Electronic photography  
Appendix X3  
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
5.1 This practice is used to assess the indigenous inclusions or second-phase constituents of metals using basic stereological procedures performed by automatic image analyzers.  
5.2 This practice is not suitable for assessing the exogenous inclusions in steels and other metals. Because of the sporadic, unpredictable nature of the distribution of exogenous inclusions, other methods involving complete inspection, for example, ultrasonics, must be used to locate their presence. The exact nature of the exogenous material can then be determined by sectioning into the suspect region followed by serial, step-wise grinding to expose the exogenous matter for identification and individual measurement. Direct size measurement rather than application of stereological methods is employed.  
5.3 Because the characteristics of the indigenous inclusion population vary within a given lot of material due to the influence of compositional fluctuations, solidification conditions and processing, the lot must be sampled statistically to assess its inclusion content. The largest lot sampled is the heat lot but smaller lots, for example, the product of an ingot, within the heat may be sampled as a separate lot. The sampling of a given lot must be adequate for the lot size and characteristics.  
5.4 The practice is suitable for assessment of the indigenous inclusions in any steel (or other metal) product regardless of its size or shape as long as enough different fields can be measured to obtain reasonable statistical confidence in the data. Because the specifics of the manufacture of the product do influence the morphological characteristics of the inclusions, the report should state the relevant manufacturing details, that is, data regarding the deformation history of the product.  
5.5 To compare the inclusion measurement results from different lots of the same or similar types of steels, or other metals, a standard sampling scheme should be adopted such as described in Practice E4...
SCOPE
1.1 This practice describes a procedure for obtaining stereological measurements that describe basic characteristics of the morphology of indigenous inclusions in steels and other metals using automatic image analysis. The practice can be applied to provide such data for any discrete second phase.  
Note 1: Stereological measurement methods are used in this practice to assess the average characteristics of inclusions or other second-phase particles on a longitudinal plane-of-polish. This information, by itself, does not produce a three-dimensional description of these constituents in space as deformation processes cause rotation and alignment of these constituents in a preferred manner. Development of such information requires measurements on three orthogonal planes and is beyond the scope of this practice.  
1.2 This practice specifically addresses the problem of producing stereological data when the features of the constituents to be measured make attainment of statistically reliable data difficult.  
1.3 This practice deals only with the recommended test methods and nothing in it should be construed as defining or establishing limits of acceptability.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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 Qualitative measurement of “nodularity” and “nodule count” using visual estimations has been practiced for many years. These methods suffer from poor reproducibility and repeatability. The introduction of computer-aided image analysis enables metallographers to measure and count individual particles of interest in a microstructure with a high degree of precision. This greatly reduces measurement variations compared to visual estimation methods (see, for example, Test Method A247).  
5.2 This method defines a procedure for measuring the number of nodules and the quality of nodularity of spherulitic graphite in a cast iron microstructure. The specimen’s location in a casting or cast test specimen, and the orientation of the plane-of-polish, are governed by product standards. When a product standard is not defined, choose the test location randomly or at specific systematically chosen depths as needed. The plane-of-polish may be parallel or perpendicular to the solidification direction, or chosen at random, depending upon the needs of the study.  
5.3 This test method may be used to determine variations within a given test specimen, within a given location in a casting, between different locations in a casting, or for the same location in different castings over time. Results from this test method may be used to qualify material for shipment in accordance with guidelines agreed upon between purchaser and manufacturer or can be used to monitor process quality or product variations.  
5.4 Measurements are performed using a computer-controlled automatic image analysis system.  
5.5 A minimum number of specimens and a minimum surface area to be evaluated may be defined by producer-purchaser agreement, provided at least 500 particles meeting the minimum size requirements are measured. The number of particles analyzed shall be indicated in the final analysis report (see 9.6).
SCOPE
1.1 This test method is used to determine the percent nodularity and the nodule count per unit area (that is, number of nodules per mm2) using a light microscopical image of graphite in nodular cast iron. Images generated by other devices, such as a scanning electron microscope, are not specifically addressed, but can be utilized if the system is calibrated in both  x and y directions.  
1.2 Measurement of secondary or temper carbon in other types of cast iron, for example, malleable cast iron or in graphitic tool steels, is not specifically included in this standard because of the different graphite shapes and sizes inherent to such grades  
1.3 This standard deals only with the recommended test method and nothing in it should be construed as defining or establishing limits of acceptability or fitness for purpose of the material tested.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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 Qualitative measurement of “nodularity” and “nodule count” using visual estimations has been practiced for many years. These methods suffer from poor reproducibility and repeatability. The introduction of computer-aided image analysis enables metallographers to measure and count individual particles of interest in a microstructure with a high degree of precision. This greatly reduces measurement variations compared to visual estimation methods (see, for example, Test Method A247).  
5.2 This method defines a procedure for measuring the number of nodules and the quality of nodularity of spherulitic graphite in a cast iron microstructure. The specimen’s location in a casting or cast test specimen, and the orientation of the plane-of-polish, are governed by product standards. When a product standard is not defined, choose the test location randomly or at specific systematically chosen depths as needed. The plane-of-polish may be parallel or perpendicular to the solidification direction, or chosen at random, depending upon the needs of the study.  
5.3 This test method may be used to determine variations within a given test specimen, within a given location in a casting, between different locations in a casting, or for the same location in different castings over time. Results from this test method may be used to qualify material for shipment in accordance with guidelines agreed upon between purchaser and manufacturer or can be used to monitor process quality or product variations.  
5.4 Measurements are performed using a computer-controlled automatic image analysis system.  
5.5 A minimum number of specimens and a minimum surface area to be evaluated may be defined by producer-purchaser agreement, provided at least 500 particles meeting the minimum size requirements are measured. The number of particles analyzed shall be indicated in the final analysis report (see 9.6).
SCOPE
1.1 This test method is used to determine the percent nodularity and the nodule count per unit area (that is, number of nodules per mm2) using a light microscopical image of graphite in nodular cast iron. Images generated by other devices, such as a scanning electron microscope, are not specifically addressed, but can be utilized if the system is calibrated in both  x and y directions.  
1.2 Measurement of secondary or temper carbon in other types of cast iron, for example, malleable cast iron or in graphitic tool steels, is not specifically included in this standard because of the different graphite shapes and sizes inherent to such grades  
1.3 This standard deals only with the recommended test method and nothing in it should be construed as defining or establishing limits of acceptability or fitness for purpose of the material tested.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
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 Hardness tests have been found to be very useful for materials evaluation, quality control of manufacturing processes and research and development efforts. Hardness, although empirical in nature, can be correlated to tensile strength for many metals and alloys, and is also an indicator of machinability, wear resistance, toughness and ductility.  
5.2 Microindentation tests are utilized to evaluate and quantify hardness variations that occur over a small distance. These variations may be intentional, such as produced by localized surface hardening, for example, from shot blasting, cold drawing, flame hardening, induction hardening, etc., or from processes such as carburization, nitriding, carbonitriding, etc.; or, they may be unintentional variations due to problems, such as decarburization, localized softening in service, or from compositional/microstructural segregation problems. Low test forces also extend hardness testing to materials too thin or too small for macroindentation tests. Microindentation tests permit hardness testing of specific phases or constituents and regions or gradients too small for evaluation by macroindentation tests.  
5.3 Because microindentation hardness tests will reveal hardness variations that commonly exist within most materials, a single test value may not be representative of the bulk hardness. Vickers tests at 1000 gf can be utilized for determination of the bulk hardness, but, as for any hardness test, it is recommended that a number of indents are made and the average and standard deviation are calculated, as needed or as required.  
5.4 Microindentation hardness testing is generally performed to quantify variations in hardness that occur over small distances. To determine these differences requires a very small physical indentation. Testers that create indents at very low test forces must be carefully constructed to accurately apply the test forces exactly at the desired location and must have a high-quality optical syste...
SCOPE
1.1 This test method covers determination of the microindentation hardness of materials.  
1.2 This test method covers microindentation tests made with Knoop and Vickers indenters under test forces in the range from 9.8 × 10-3 to 9.8 N (1 to 1000 gf).  
1.3 This test method includes an analysis of the possible sources of errors that can occur during microindentation testing and how these factors affect the precision, bias, repeatability, and reproducibility of test results.  
1.4 Information pertaining to the requirements for direct verification and calibration of the testing machine and the requirements for the manufacture and calibration of Vickers and Knoop reference hardness test blocks are in Test Method E92.
Note 1: While Committee E04 is primarily concerned with metals, the test procedures described are applicable to other materials.  
1.5 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 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 This practice is used to assess the nature and extent of banding or orientation of microstructures of metals and other materials where deformation and processing produce a banded or oriented condition.  
5.2 Banded or oriented microstructures can arise in single phase, two phase or multiphase metals and materials. The appearance of the orientation or banding is influenced by processing factors such as the solidification rate, the extent of segregation, the degree of hot or cold working, the nature of the deformation process used, the heat treatments, and so forth.  
5.3 Microstructural banding or orientation influence the uniformity of mechanical properties determined in various test directions with respect to the deformation direction.  
5.4 The stereological methods can be applied to measure the nature and extent of microstructural banding or orientation for any metal or material. The microindentation hardness test procedure should only be used to determine the difference in hardness in banded heat-treated metals, chiefly steels.  
5.5 Isolated segregation may also be present in an otherwise reasonably homogeneous microstructure. Stereological methods are not suitable for measuring individual features, instead use standard measurement procedures to define the feature size. The microindentation hardness method may be used for such structures.  
5.6 Results from these test methods may be used to qualify material for shipment in accordance with guidelines agreed upon between purchaser and manufacturer, for comparison of different manufacturing processes or process variations, or to provide data for structure-property-behavior studies.
SCOPE
1.1 This practice describes a procedure to qualitatively describe the nature of banded or oriented microstructures based on the morphological appearance of the microstructure.  
1.2 This practice describes stereological procedures for quantitative measurement of the degree of microstructural banding or orientation.  
Note 1: Although stereological measurement methods are used to assess the degree of banding or alignment, the measurements are only made on planes parallel to the deformation direction (that is, a longitudinal plane) and the three-dimensional characteristics of the banding or alignment are not evaluated.  
1.3 This practice describes a microindentation hardness test procedure for assessing the magnitude of the hardness differences present in banded heat-treated steels. For fully martensitic carbon and alloy steels (0.10–0.65 %C), in the as-quenched condition, the carbon content of the matrix and segregate may be estimated from the microindentation hardness values.  
1.4 This standard does not cover chemical analytical methods for evaluating banded structures.  
1.5 This practice deals only with the recommended test methods and nothing in it should be construed as defining or establishing limits of acceptability.  
1.6 The measured values are stated in SI units, which are regarded as standard. Equivalent inch-pound values, when listed, are in parentheses and may be approximate.  
1.7 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.

SIGNIFICANCE AND USE
4.1 The presence of large grains has been correlated with anomalous mechanical behavior in, for example, crack initiation, crack propagation, and fatigue. Thus there is engineering justification for reporting the ALA grain size.  
4.2 These methods shall only be used with the presence of outlier coarse grains, 3 or more ASTM grain size numbers larger than the rest of the microstructure and comprising 5 % or less of the specimen area. A typical example is shown in Annex A1 as Fig. A1.1.  
4.3 These methods shall not be used for the determination of average grain size, which is treated in Test Methods E112. Examples of microstructures that do not qualify for ALA treatment are shown in Annex A1 as Fig. A1.2, Fig. A1.3, and Fig. A1.4.  
4.4 These methods may be applied in the characterization of duplex grain sizes, as instructed in the procedures for Test Methods E1181.
SCOPE
1.1 These test methods describe simple manual procedures for measuring the size of the largest grain cross-section observed on a metallographically prepared plane section.  
1.2 These test methods shall only be valid for microstructures containing outlier coarse grains, where their population is too sparse for grain size determination by Test Methods E112.  
1.3 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.

SIGNIFICANCE AND USE
5.1 These test methods cover procedures for determining the mean grain size, and the distribution of grain intercept lengths or grain areas, for polycrystalline metals and nonmetallic materials with equiaxed or deformed grain shapes, with uniform or duplex grain size distributions, and for single phase or multiphase grain structures.  
5.2 The measurements are performed using semiautomatic digitizing tablet image analyzers or automatic image analyzers. These devices relieve much of the tedium associated with manual measurements, thus permitting collection of a larger amount of data and more extensive sampling which will produce better statistical definition of the grain size than by manual methods.  
5.3 The precision and relative accuracy of the test results depend on the representativeness of the specimen or specimens, quality of specimen preparation, clarity of the grain boundaries (etch technique and etchant used), the number of grains measured or the measurement area, errors in detecting grain boundaries or grain interiors, errors due to detecting other features (carbides, inclusions, twin boundaries, and so forth), the representativeness of the fields measured, and programming errors.  
5.4 Results from these test methods may be used to qualify material for shipment in accordance with guidelines agreed upon between purchaser and manufacturer, to compare different manufacturing processes or process variations, or to provide data for structure-property-behavior studies.
SCOPE
1.1 These test methods are used to determine grain size from measurements of grain intercept lengths, intercept counts, intersection counts, grain boundary length, and grain areas.  
1.2 These measurements are made with a semiautomatic digitizing tablet or by automatic image analysis using an image of the grain structure produced by a microscope.  
1.3 These test methods are applicable to any type of grain structure or grain size distribution as long as the grain boundaries can be clearly delineated by etching and subsequent image processing, if necessary.  
1.4 These test methods are applicable to measurement of other grain-like microstructures, such as cell structures.  
1.5 This standard deals only with the recommended test methods and nothing in it should be construed as defining or establishing limits of acceptability or fitness for purpose of the materials tested.  
1.6 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.  
1.7 The sections appear in the following order:    
Section  
Section  
Scope  
1  
Referenced Documents  
2  
Terminology  
3  
Definitions  
3.1  
Definitions of Terms Specific to This Standard  
3.2  
Symbols  
3.3  
Summary of Test Method  
4  
Significance and Use  
5  
Interferences  
6  
Apparatus  
7  
Sampling  
8  
Test Specimens  
9  
Specimen Preparation  
10  
Calibration  
11  
Procedure:  
Semiautomatic Digitizing Tablet  
12  
Intercept Lengths  
12.3  
Intercept and Intersection Counts  
12.4  
Grain Counts  
12.5  
Grain Areas  
12.6  
ALA Grain Size  
12.6.1  
Two-Phase Grain Structures  
12.7  
Procedure:  
Automatic Image Analysis  
13  
Grain Boundary Length  
13.5  
Intersection Counts  
13.6  
Mean Chord (Intercept) Length/Field  
13.7.2  
Individual Chord (Intercept) Lengths  
13.7.4  
Grain Counts  
13.8  
Mean Grain Area/Field  
13.9  
Individual Grain Areas  
13.9.4  
ALA Grain Size  
13.9.8  
Two-Phase Grain Structures  
13.10  
Calculation of Results  
14  
Test Report  
15  
Precision and Bias  
16  
Grain Size of Non-Equiaxed Grain Structure Specimens  
Annex A1  
Examples...