E04.11 - X-Ray and Electron 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
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
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
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.
SCOPE
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.

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.
SCOPE
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
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.
SCOPE
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 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
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 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
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 and health practices and determine the applicability of regulatory limitations prior to use.

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

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.
SCOPE
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 and health practices and determine the applicability of regulatory limitations prior to use.

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.
SCOPE
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 and health practices and determine the applicability of regulatory limitations prior to use.

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.
SCOPE
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 and health practices and determine the applicability of regulatory limitations prior to use.

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 sample 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 practice 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 practice 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 and health practices and determine the applicability of regulatory limitations prior to use.TABLE 1 Calculated Theoretical Intensities Using Chromium Kα  RadiationA    
hkl  
Sinθ/λ  
θ  
f  
Δf′  
Δf"  
/F/2  
LP  
P  
TB  
N2  
R  
(α iron, body-centered cubic, unit-cell dimension ao  = 2.8664Å):    
110  
0.24669  
34.41  
18.474  
−1.6  
0.9  
1142.2  
4.290  
12  
0.9577  
0.001803B  
101.5C  
200  
0.34887  
53.06  
15.218  
−1.6  
0.9  
745.0  
2.805  
6  
0.9172  
0.001803B  
20.73C  
211  
0.42728  
78.20  
13.133  
−1.6  
0.8  
534.6  
9.388  
24  
0.8784  
0.001803B  
190.8C  
(γ iron, face-centered cubic, unit-cell dimension a o  = 3.60Å):  
111  
0.24056  
33.44  
18.687  
−1.6  
0.9  
4684.4  
4.554  
8  
0.9597  
0.0004594B  
75.24C  
200  
0.27778  
39.52  
17.422  
−1.6  
0.9  
4018.3  
3.317  
6  
0.9467  
0.0004594B  
34.78C  
220  
0.39284  
64.15  
14.004  
−1.6  
0.8  
2472.0  
3.920  
12  
0.8962  
0.0004594B  
47.88C A Data from “International Tables for X-Ray Crystallography,” Physical and Chemical Tables , Vol III, Kynoch Press, Birmingham, England, 1962, pp. 60, 61, 210, 213; Weighted Kα1  and  Kα2  value used (λ = 2.29092Å).B Temperature factor (T = e−2M) where M = B(sin 2 θ)/λ2  and 2B = 0.71. Also N is the reciprocal of the unit-cell volume. C Calculated intensity includes the variables listed that change with X-ray diffraction peak position.

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.
SCOPE
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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
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.
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 1.0 %,2 can be analyzed but with lower precision compared with analyses of elements present in greater concentration.
SCOPE
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. 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
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.
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) 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.

SIGNIFICANCE AND USE
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.
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.

SIGNIFICANCE AND USE
This practice can be used to extract carbides, borides, TCP and GCP phases, which can then be qualitatively or quantitatively analyzed by X-ray diffraction or microanalysis.  
Careful control of parameters is necessary for reproducible quantitative results. Within a given laboratory, such results can be obtained routinely; however, caution must be exercised when comparing quantitative results from different laboratories.  
Comparable qualitative results can be obtained routinely among different laboratories using this procedure.
SCOPE
1.1 This practice covers a procedure for the isolation of carbides, borides, TCP (topologically close-packed), and GCP (geometrically close-packed) phases (Note 1) in nickel and nickel-iron base gamma prime strengthened alloys. Contamination of the extracted residue by coarse matrix (gamma) or gamma prime particles, or both, reflects the condition of the alloy rather than the techniques mentioned in this procedure.
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
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.
SCOPE
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 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.

SIGNIFICANCE AND USE
Metals and other materials are not always isotropic in their physical properties. For example, Young's modulus will vary in different crystallographic directions. Therefore, it is desirable or necessary to determine the orientation of a single crystal undergoing tests in order to ascertain the relation of any property to different directions in the material.
This test method can be used commercially as a quality control test in production situations where a desired orientation, within prescribed limits, is required.
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.
If grains of a polycrystalline material are large enough, this test method can be used to determine their orientations and differences in orientation.
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 (1, 2) may be applied to macrograins (3) (0.5-mm diameter or larger) within polycrystalline aggregates, as well as to single crystals of any size. The method is described with reference to cubic crystals; it can be applied equally well to 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) must 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 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.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
This test method is established to cover automated SEM/EDX-based procedures for:
Rating the inclusion content of steels based on procedures listed in Standards E 45 and E 1245, 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.
Determining the number, size and morphological distribution of inclusions in steels sorted by chemical class.
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).
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 E 45), and in tabulated in Table 2. Test Method E 45 ratings by SEM may differ from those determined following E 45 because of the use of chemistry in the classifications. In order to differentiate E 45 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 E 45-SEM1 and E 45-SEM2, respectively.
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.
Method 3 determines and reports basic (as used in Test Method E 1245) stereological measurements (for example, volume fraction of sulfides and oxides, the number of sulfides or oxides per square millimeter, and so forth). T...
SCOPE
1.1 This test method covers procedures to obtain particle size distribution, chemical classification, and Test Methods E 45 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 E 45, which uses image analysis and light microscopy to produce automated Test Methods E 45 ratings. Method 2 produces similar ratings based predominantly on sorting inclusions by chemistry into the traditional classes defined in Test Methods E 45. Method 3 is recommended when explicit detail is needed on particular inclusion types, not necessarily defined in Test Methods E 45, 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 E 45 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
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.
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.
The accuracy of the calibrated magnifications, or dimensional measurements, will be poorer than the accuracy of the calibration specimen used with this practice.
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.
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.
SCOPE
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. 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
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.
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 sample 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 practice 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 practice 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. 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
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.
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 1.0 %,2 can be analyzed but with lower precision compared with analyses of elements present in greater concentration.
SCOPE
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. 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
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.
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) 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.

SIGNIFICANCE AND USE
Metals and other materials are not always isotropic in their physical properties. For example, Young’modulus will vary in different crystallographic directions. Therefore, it is desirable or necessary to determine the orientation of a single crystal undergoing tests in order to ascertain the relation of any property to different directions in the material.
This test method can be used commercially as a quality control test in production situations where a desired orientation, within prescribed limits, is required.
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.
If grains of a polycrystalline material are large enough, this test method can be used to determine their orientations and differences in orientation.
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 (1, 2) may be applied to macrograins (3) (0.5-mm diameter or larger) within polycrystalline aggregates, as well as to single crystals of any size. The method is described with reference to cubic crystals; it can be applied equally well to 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) must 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 The values stated in inch-pound units are to be regarded as 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
This practice can be used to extract carbides, borides, TCP and GCP phases, which can then be qualitatively or quantitatively analyzed by X-ray diffraction or microanalysis.2  
Careful control of parameters is necessary for reproducible quantitative results. Within a given laboratory, such results can be obtained routinely; however, caution must be exercised when comparing quantitative results from different laboratories.3  
Comparable qualitative results can be obtained routinely among different laboratories using this procedure.3
SCOPE
1.1 This practice covers a procedure for the isolation of carbides, borides, TCP (topologically close-packed), and GCP (geometrically close-packed) phases (Note 0) in nickel and nickel-iron base gamma prime strengthened alloys. Contamination of the extracted residue by coarse matrix (gamma) or gamma prime particles, or both, reflects the condition of the alloy rather than the techniques mentioned in this procedure.
This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. (See 3.3.2.1 and 4.1.1.)
Note 1
Ni3 Ti (eta phase) has been found to be soluble in the electrolyte for some alloys.

SIGNIFICANCE AND USE
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.
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 x. 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.

SIGNIFICANCE AND USE
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.
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 sample 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 practice covers the determination of retained austenite phase in steel using integrated intensities (area under peak above background) of X-ray diffraction peaks using chromium  K  or molybdenum K 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 practice 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 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
This 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.
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 1.0 %,2 can be analyzed but with lower precision compared with analyses of elements present in greater concentration.
SCOPE
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. This guide does not cover EDS with a transmission electron microscope (TEM).
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
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.
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.
The accuracy of the calibrated magnifications, or dimensional measurements, will be poorer than the accuracy of the calibration specimen used with this practice.
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.
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.
SCOPE
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. 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 the standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SCOPE
1.1 This test method covers procedures to obtain particle size distribution, chemical classification, and 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 E1122, which uses image analysis and light microscopy to produce automated E45 ratings. Method 2 produces similar ratings based predominantly on sorting inclusions by chemistry into the traditional classes defined in E45. Method 3 is recommended when explicit detail is needed on particular inclusion types, not necessarily defined in E 45, 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 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 the standard. Values in parentheses are conversions and are approximate, and for information only.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SCOPE
1.1 This 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) 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 ori- entation 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.

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) 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 ori- entation 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.

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 (1, 2) may be applied to macrograins (3) (0.5-mm diameter or larger) within polycrystalline aggregates, as well as to single crystals of any size. The method is described with reference to cubic crystals; it can be applied equally well to 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) must 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 The values stated in inch-pound units are to be regarded as the standard.  
1.4 This standard does not purport to address the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SCOPE
1.1 This 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 (1, 2) may be applied to macrograins (3) (0.5-mm diameter or larger) within polycrystalline aggregates, as well as to single crystals of any size. The method is described with reference to cubic crystals; it can be applied equally well to 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) must 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 The values stated in inch-pound units are to be regarded as the standard.  
1.4 This standard does not purport to address the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SCOPE
1.1 This practice covers the determination of retained austenite phase in steel using integrated intensities (area under peak above background) of X-ray diffraction peaks using chromium K[alpha] or molybdenum K[alpha] 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 practice 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 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SCOPE
1.1 This practice covers a procedure for the isolation of carbides, borides, TCP (topologically close-packed), and GCP (geometrically close-packed) phases (Note 1) in nickel and nickel-iron base gamma prime strengthened alloys. Contamination of the extracted residue by coarse matrix (gamma) or gamma prime particles, or both, reflects the condition of the alloy rather than the techniques mentioned in this procedure.  
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. (See 3.3.2.1 and 4.1.1.)
Note 1--Ni3 Ti (eta phase) has been found to be soluble in the electrolyte for some alloys.

SCOPE
1.1 This practice covers a procedure for the isolation of carbides, borides, TCP (topologically close-packed), and GCP (geometrically close-packed) phases (Note 1) in nickel and nickel-iron base gamma prime strengthened alloys. Contamination of the extracted residue by coarse matrix (gamma) or gamma prime particles, or both, reflects the condition of the alloy rather than the techniques mentioned in this procedure.  
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. (See 3.3.2.1 and 4.1.1.)
Note 1--Ni3 Ti (eta phase) has been found to be soluble in the electrolyte for some alloys.

SCOPE
1.1 This practice is designed to calibrate the magnification of scanning electron microscopes (SEMs) using the National Institute of Standards and Technology (NIST) calibration specimen Standard Reference Material (SRM)484. Since the relationship between true magnification and magnification indicated on the SEM readout may be different at different magnifications, this practice must be applied to each magnification for which true magnification is desired.
1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SCOPE
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.  This guide does not cover EDS with a transmission electron microscope (TEM).
1.2 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SCOPE
1.1 This practice provides a reproducible means by which the performance of a scanning electron microscope (SEM) may be characterized. This performance is a measure of the SEM-operator-material combination and is 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, -deflection waveform generation) for the suggested materials. The range of SEM magnification at which this practice is of utility is from 1000 to 200 000 X.  
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
3.1 This practice can be used to extract carbides, borides, TCP and GCP phases, which can then be qualitatively or quantitatively analyzed by X-ray diffraction or microanalysis.2  
3.2 Careful control of parameters is necessary for reproducible quantitative results. Within a given laboratory, such results can be obtained routinely; however, caution must be exercised when comparing quantitative results from different laboratories.3  
3.3 Comparable qualitative results can be obtained routinely among different laboratories using this procedure.3
SCOPE
1.1 This practice covers a procedure for the isolation of carbides, borides, TCP (topologically close-packed), and GCP (geometrically close-packed) phases (Note 1) in nickel and nickel-iron base gamma prime strengthened alloys. Contamination of the extracted residue by coarse matrix (gamma) or gamma prime particles, or both, reflects the condition of the alloy rather than the techniques mentioned in this procedure.  
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. (See 4.3.2.1 and 5.1.1.)  
Note 1: Ni3 Ti (eta phase) has been found to be soluble in the electrolyte for some alloys.  
FIG. 1 Schematic Diagram of Extraction Cell
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.
WITHDRAWN RATIONALE
This practice covers a procedure for the isolation of carbides, borides, TCP (topologically close-packed), and GCP (geometrically close-packed) phases (Note 1) in nickel and nickel-iron base gamma prime strengthened alloys. Contamination of the extracted residue by coarse matrix (gamma) or gamma prime particles, or both, reflects the condition of the alloy rather than the techniques mentioned in this procedure.
Formerly under the jurisdiction of Committee E04 on Metallography, this practice was withdrawn in May 2018. This standard is being withdrawn without replacement due to its limited use by industry.