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Astm E45 PDF
Astm E45 PDF
required, either a macroscopic or a microscopic method for AMS 2300, Premium Aircraft-Quality Steel Cleanliness:
determining the inclusion content, or combinations of the two Magnetic Particle Inspection Procedure
methods, may be found most satisfactory. AMS 2301, Aircraft Quality Steel Cleanliness: Magnetic
1.4 These test methods deal only with recommended test Particle Inspection Procedure
methods and nothing in them should be construed as defining AMS 2303, Aircraft Quality Steel Cleanliness: Martensitic
or establishing limits of acceptability for any grade of steel. Corrosion-Resistant Steels Magnetic Particle Inspection
1.5 The values stated in SI units are to be regarded as the Procedure
standard. Values in parentheses are conversions and are ap- AMS 2304, Special Aircraft-Quality Steel Cleanliness:
proximate. Magnetic Particle Inspection Procedure
1.6 This standard does not purport to address all of the 2.4 ISO Standards:4
safety concerns, if any, associated with its use. It is the ISO 3763, Wrought Steels—Macroscopic Methods for As-
responsibility of the user of this standard to establish appro- sessing the Content of Nonmetallic Inclusions
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
1
These test methods are under the jurisdiction of ASTM Committee E04 on the ASTM website.
3
Metallography and is the direct responsibility of Subcommittee E04.09 on Inclu- Available from Society of Automotive Engineers (SAE), 400 Commonwealth
sions. Dr., Warrendale, PA 15096-0001.
4
Current edition approved Nov. 1, 2005. Published December 2005. Originally Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
approved in 1942. Last previous edition approved in 2002 as E 45 – 97 (2002). 4th Floor, New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
Methods A and D of these test methods are the principal JK oped by these methods can be found in ASTM product
rating methods, and Method E also uses the JK rating charts. standards or may be described by purchaser-producer agree-
3.2.5 stringer—an individual inclusion that is highly elon- ments. By agreements between producer and purchaser, this
gated in the deformation direction or three or more Type B or practice may be modified to count only certain inclusion types
C inclusions aligned in a plane parallel to the hot working axis and thicknesses, or only those inclusions above a certain
and offset by no more than 15 µm, with a separation of less than severity level, or both. Also, by agreement, qualitative prac-
40 µm (0.0016 in.) between any two nearest neighbor inclu- tices may be used where only the highest severity ratings for
sions. each inclusion type and thickness are defined or the number of
3.2.6 threshold setting—isolation of a range of gray level fields containing these highest severity ratings are tabulated.
values exhibited by one constituent in the microscope field. 4.7 These test methods are intended for use on wrought
3.2.7 worst-field rating—a rating in which the specimen is metallic structures. While a minimum level of deformation is
rated for each type of inclusion by assigning the value for the not specified, the test methods are not suitable for use on cast
highest severity rating observed of that inclusion type any- structures or on lightly worked structures.
where on the specimen surface.
4.8 Guidelines are provided to rate inclusions in steels
4. Significance and Use treated with rare earth additions or calcium-bearing com-
pounds. When such steels are evaluated, the test report should
4.1 These test methods cover four macroscopic and five
describe the nature of the inclusions rated according to each
microscopic test methods (manual and image analysis) for
inclusion category (A, B, C, D).
describing the inclusion content of steel and procedures for
expressing test results. 4.9 In addition to the Practice E 45 JK ratings, basic (such
4.2 Inclusions are characterized by size, shape, concentra- as used in Practice E 1245) stereological measurements (for
tion, and distribution rather than chemical composition. Al- example, the volume fraction of sulfides and oxides, the
though compositions are not identified, Microscopic methods number of sulfides or oxides per square millimeter, the spacing
between inclusions, and so forth) may be separately deter-
mined and added to the test report, if desired for additional
5
Available from ASTM Headquarters. Order ADJE004502. information. This practice, however, does not address the
6
Available from ASTM Headquarters. Order ADJE004501. measurement of such parameters.
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sampling should involve a greater number of test specimens for should be invoked.
an equivalent weight of steel. A value for the inclusion content 7.2 For cases in which a definite location within a heat,
of an isolated piece of steel, even if accurately determined, ingot, or other unit lot is unknown, statistical random sampling
should not be expected to represent the inclusion content of the with a greater number of specimens should be employed.
whole heat. 7.3 Ratings obtained will vary with the amount of reduction
6.9 The size and shape of the wrought steel product tested of the product. For materials acceptance or for comparison
has a marked influence on the size and shape of the inclusions. among heats, care must be taken to sample at the correct stage
During reduction from the cast shape by rolling or forging, the of processing.
inclusions are elongated and broken up according to the degree
of reduction of the steel cross section. In reporting results of 8. Test Specimen Geometry
inclusion determinations, therefore, the size, shape, and 8.1 The minimum polished surface area of a specimen for
method of manufacture of the steel from which the specimens the microscopic determination of inclusion content is 160
were cut must be stated. In comparing the inclusion content of mm2 (0.25 in.2). It is recommended that a significantly large
different steels, they must all be rolled or forged as nearly as area should be obtained so that the measurements may be made
possible to the same size and shape, and from cast sections of within the defined area away from the edges of the sample. The
about the same size. Specimens cut lengthwise or parallel to polished surface must be parallel to the longitudinal axis of the
the direction of rolling or forging shall be used. product. In addition, for flat-rolled products, the section shall
6.10 It may be convenient, in order to obtain more readily also be perpendicular to the rolling plane; for rounds and
comparable results, to forge coupons from larger billets. These tubular shapes, the section shall be in the radial direction. In all
forged sections may then be sampled in the same way as rolled cases, the polished surface shall be parallel to the hot-working
disk at least 12 mm (0.474 in.) thick is cut from the product. size from which specimens should be taken; however, larger or
The quarter-section indicated in Fig. 3 is cut from the disk and smaller sizes may be used, provided the product sizes are
the shaded area is polished. Thus the specimen extends at least reported with the results.
12 mm along the length of the product from the outside to the 8.3 Thin Sections (Product Section Sizes 9.5 mm (0.375 in.)
center. Thick or Less; Strip, Sheet, Rod, Wire, and Tubing)—Full cross
8.2.3 For large sections, each specimen shall be taken from section longitudinal specimens shall be cut in accordance with
the mid-radius location, as shown by the shaded area in Fig. 4. the following plan:
The specimen face to be polished extends at least 12 mm 8.3.1 For 0.95 to 9.5-mm (0.0375 to 0.375 in.) cross section
parallel to the longitudinal axis of the billet and at least 19 mm thicknesses inclusively, a sufficient number of pieces from the
(0.75 in.) in the longitudinal radial plane, with the polished same sampling point are mounted to provide approximately
face midway between the center and the outside of the billet. 160 mm2 (0.25 in.2) of polished specimen surface. (Example:
Such midway sampling is used to decrease the number of For a sheet 1.27 mm (0.050 in.) thick, select seven or eight
longitudinal pieces uniformly across the sheet width to provide
one specimen).
9
Allmand, T. R., and Coleman, D. S., “The Effect of Sectioning Errors on
8.3.2 For cross section thicknesses less than 0.95 mm, ten
Microscopic Determinations of Non-Metallic Inclusions in Steels,” Metals and longitudinal pieces from each sampling location shall be
Materials, Vol 7, 1973, pp. 280–283. mounted to provide a suitable specimen surface for polishing.
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mens must be examined in the as-polished condition, free from detected (discriminated) image, over a number of test fields, to
the effects of any prior etching (if used). ensure that the settings are correct, that is, detection of sulfides
9.2 Metallographic specimen preparation must be carefully or oxides by type and size is correct.
controlled to produce acceptable quality surfaces for both
manual and image analysis. Guidelines and recommendations 11. Classification of Inclusions and Calculation of
are given in Practice E 3, Test Methods E 45, and Practice Severities
E 768. 11.1 In these microscopic methods, inclusions are classified
9.3 Inclusion retention is generally easier to accomplish in into four categories (called Type) based on their morphology
hardened steel specimens than in the annealed condition. If and two subcategories based on their width or diameter.
inclusion retention is inadequate in annealed specimens, they Categories A-Sulfide Type, B-Alumina Type, C-Silicate Type
should be subjected to a standard heat treatment cycle using a and D-Globular Oxide Type define their shape while categories
relatively low tempering temperature. After heat treatment, the Heavy and Thin describe their thickness. Although the catego-
specimen must be descaled and the longitudinal plane must be ries contain chemical names that imply knowledge of their
reground below any decarburization. This recommendation chemical content, the ratings are based strictly on morphology.
only applies to heat-treatable steel grades. The chemical names associated with the various Types were
9.4 Mounting of specimens is not required if unmounted derived from historical data collected on inclusions found in
specimens can be properly polished. these shapes or morphologies. The four categories, or Types,
are partitioned into Severity Levels based on the number or
10. Calibration and Standardization length of the particles present in a 0.50 mm2 field of view.
10.1 Recommended calibration guidelines can be found in These Severity Levels and inclusion Types are depicted in
Guide E 1951. Plate I-r and their numerical equivalents are found in Tables 1
10.2 For image analysis, a stage micrometer and a ruler, and 2.
both calibrated against devices traceable to a recognized 11.1.1 Type A and C inclusions are very similar in size and
national standards laboratory, such as the National Institute for shape. Therefore, discrimination between these Types is aided
Standards and Technology (NIST), are used to determine the by metallographic techniques. Type A-Sulfide are light gray
magnification of the system and calibrate the system in while Type C-Silicate are black when viewed under brightfield
accordance with the manufacturer’s recommended procedure. illumination. Discrimination between these types may also be
For example, the ruler is superimposed over the magnified aided by viewing the questionable inclusions under darkfield or
image of the stage micrometer on the monitor. The apparent cross-polarized illumination where properly polished sulfide
(magnified) distance between two known points on the stage inclusions are dark and silicate inclusions appear luminescent.
micrometer is measured with the ruler. The magnified distance 11.2 The B-type stringers consist of a number (at least three)
is divided by the true distance to determine the screen of round or angular oxide particles with aspect ratios less than
magnification. The pixel dimensions can be determined from 2 that are aligned nearly parallel to the deformation axis.
the number of pixels for a known horizontal or vertical Particles within 615 µm of the centerline of a B-type stringer
dimension on the monitor. Divide the known length of a scale are considered to be part of that stringer. The Type C-Silicate
or mask by the number of pixels representing that length on the stringers consist of one or more highly elongated oxides with
monitor to determine the pixel size for each possible screen smooth surfaces aligned parallel to the deformation axis.
magnification. Not all systems use square pixels. Determine the Aspect ratios are generally high, $ 2. The maximum permitted
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NOTE 1—The square mask will yield a field area of 0.50 mm2 on the specimen surface. A graphic representation of the maximum thickness of the Thin
and Heavy series of Types A, B, C, and D is on the left. Several oversized Type D are depicted on the right for convenience.
FIG. 5 Suggested Reticle or Overlay Grid For Methods A, D, and E
NOTE 1—Systematically scan the entire masked area. Methods A, B, C, and E permit adjustment of the field locations in order to maximize a severity
level number or facilitate a measurement. For Method D, the fields must remain contiguous and only features within the field are compared to Plate I-r.
NOTE 2—Method D will require a larger (10 3 17 mm) test area to facilitate placement of enough contiguous, 0.71 mm square fields to total 160 mm2
of polished surface area.
FIG. 6 Typical Scan Pattern for Microscopic Methods
inclusion or inclusion stringer still contributes to the determi- appear at the bottom of Plate I-r. A Type D globular oxide may
nation of a field’s Severity Level Number. Therefore, if an A, not exceed an aspect ratio of 2:1.
B, or C inclusion is oversized either in length or thickness that 11.9 Oxides located at the tips of Type A-Sulfide inclusions
portion that is within the field boundaries shall be included in are rated at Type D- Globular Oxides unless they are close
the appropriate Thin or Heavy severity level measurement. enough together to meet the requirements of a Type
Likewise, if an oversize D inclusion is encountered in a field, B-Alumina.
it is also included in the count that determines the D heavy 11.10 The indigenous inclusions in steels deoxidized with
rating. For reference, illustrations of large, globular oxides rare earth elements or calcium-containing materials are also
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composition must be provided to avoid confusion. Because to report severity levels > 3.0). Do this for both the Thin and
they are sulfides with a D-type morphology, they may be Heavy series. It is important to note here that if a field of
referred to as DS. inclusions falls between two severity levels, its value is
rounded down to the lower severity level. For example, when
11.11 Complex inclusions, such as oxysulfides or duplex
using Plate I-r, a field that contains fewer inclusions, or less
inclusions, are also rated according to their morphology:
inclusion length than Severity Level Number 1, is counted as a
whether they are stringered or elongated (for aspect ratios $ 2)
0.
or isolated (not part of a stringer and aspect ratio < 2); and then
12.2.3 Move the microscope stage to reveal an adjacent field
by thickness. Isolated, globular particles are rated as D-types
and repeat the comparison procedure. Continue this process
by their average thickness. Complex Ds may be predominantly
until the required polished surface area of the specimen has
(>50 % by area) sulfides or oxides and should be identified as
been scanned. A typical scan configuration is shown in Fig. 6.
such. For example, if the oxide area is greater in a globular
This method requires adjustment of the microscope stage to
oxysulfide, it could be called a DOS type. Stringered complex
maximize an inclusion severity level. That is, the field of view
particles are rated by the aspect ratio of the individual particles;
is adjusted using the microscope stage controls, such that
if < 2, they are B-types, if $ 2 they are A- or C-types (separate
inclusions are moved inside the square mask in order to locate
by gray level). For those complex inclusions with aspect ratios
the worst field. In practice, the rater is actually scanning the
$ 2, they are classified as A-types if more than 50 % of the
specimen and stopping only when a potential worst field of
area is sulfide and C-types if more than 50 % of the area is
each type and thickness is in view.
oxide. Report the composition, in general terms, to avoid
12.3 Manual Expression of Results:
confusion, and state the nature of the inclusions, for example,
12.3.1 The averages of the worst fields for each inclusion
“globular calcium aluminates encapsulated with a thin film of
type in all the specimens of the lot shall be calculated in
calcium-manganese sulfide,” or “irregular aluminates partially
accordance with the Severity Level Numbers given at the sides
or fully embedded in manganese sulfide stringers.”
of Plate I-r or Table 1. An example showing the averages
11.12 If producer-purchaser agreements limit the analysis to obtained for six specimens examined is given in Table 4.
only certain inclusion types, thickness categories, or severity 12.3.2 Oversize inclusions with widths or diameters greater
limits, the scheme in Section 11 can be modified to analyze, than the limiting values shown on Plate I-r (and Table 2) shall
measure, and store only the data of interest. It may also contain be recorded separately.
procedures to perform basic (see Practice E 1245) stereological
measurements to supplement the JK analyses. Such measure-
ments are not covered by this practice. 11
This method is similar to the Jernkontoret Method, Uppsala, Sweden (1936).
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FIG. 8 Designation of Length and Weight of Inclusions (4 Units Long)
FIG. 11 Relationship between Severity Rating and the Minimum FIG. 12 Relationship between Severity Rating and the Minimum
Total B-Type Stringer Length for Plate I-r and Table 1 Total C-Type Stringer Length for Plate I-r and Table 1
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TABLE 5 SAM Rating (Method E) results. The magnification chosen should produce a maximum
B-Type ratingA,B D-Type RatingA,C calibration factor of 1.3 microns at 1003.
No. of No. of No. of 12.5.4 Select the gray-level threshold settings to permit
“B” “B” “D”
Observed Observed Observed Units independent detection of sulfides and oxides (see 10.2.2).
Thin Heavy Heavy
Fields Fields Fields
12.5.5 When detecting sulfides, a false image (called the
not recorded 0.5 not recorded 0.5 5 0.5 (1)
not recorded 1.0 2 1.0 2 1.0 (2)
halo effect) may be detected around the periphery of oxides in
3 1.5 1 1.5 1 1.5 (3) the same field. This problem can be corrected by the use of an
1 2.0 0 2.0 0 2.0 (4) auto-delineation feature or by application of appropriate algo-
0 2.5 0 2.5 0 2.5 (5)
rithms to the binary image. Choice of the most satisfactory
A
Total area observed = 1.5 in.2 approach depends upon the image analysis system used.
B
SAM rating = (3 3 1.5) + (1 3 2) + (2 3 1) + (1 3 1.5) = 10 4 1.5 = 7.
C
SAM rating = (5 3 1) + (2 3 2) + (1 3 3) = 124 1.5 = 8. 12.5.6 Set the stage controls to move the specimen in a
square or rectangular pattern with contiguous field alignment
so that a minimum of 160 mm2 is examined and evaluated.
possible. A deviation of less than 60.05 mm2 from the required Other measurement areas may be used based on producer-
0.50-mm2 area will not significantly impair measurement purchaser agreements.
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C Log(Sev.) = [0.479731Log(C)] − 0.393723
D Log(Sev.) = [0.5Log(D)] − 0.45154
and D) and thickness (thin and thick) are reported for each indexing of fields.
severity from 0 to 5 in whole or half-severity level increments.
For steels with very low inclusion contents, severities may be 13.2.2 To begin, outline the required test area on the
computed to one-quarter or one-tenth severity level incre- specimen surface using either an indelible marker or a carbide-
ments. Note that for D-type inclusions, because one inclusion tipped scribe. Place the specimen on the microscope and start
per field is a severity of 0.5, by definition, there can be no the examination with a field in one of the corners of the marked
D-severity levels between 0 and 0.5. test area. Measure and record all inclusions in this field that are
12.6.2 If desired, based on producer-purchaser agreements, one unit long or longer. Inclusions separated by a distance
modifications of the reported data may be made, for example, greater than one unit shall be classified as two inclusions and
reports for only certain inclusion types, thicknesses, or severity not be considered as one stringer. The length of an inclusion
values. Other modifications may include only worst-field shall be rounded down to the next whole unit and only whole
severity ratings or the number of fields at the worst-field units will be recorded. For example, if an inclusion measures
severity ratings. 21⁄2 units, it shall be recorded as a “2.” If an inclusion lies
12.6.3 If desired by producer-purchaser agreement, an index partially outside of the field, that is, part of its length lies in
may be calculated to describe the inclusion content. what will become Field Number 2, move the field slightly in
12.6.4 To produce average results for more than one speci- order that its entire length may be measured.
men per lot, the average number of fields for each severity 13.2.3 Move the microscope stage to view an adjacent field.
rating, inclusion type, and thickness may be calculated (see Repeat the measurement procedure. Take care that any inclu-
Table 4). sion measured in the previous field is not remeasured. Continue
12.6.5 Data for inclusions or stringers that are oversized in this process until the required polished surface area of the
either length or width, or both, should be reported separately. specimen has been scanned. A typical scan configuration is
Report the inclusion type, measured width, and length (for shown in Fig. 6.
Types A, B, and C).
12.6.6 Fields with zero severity levels may be further 13.3 Expression of Results:
classified, if desired, as either blank (no inclusions of a 13.3.1 The determination for each specimen shall be di-
particular type and width category are present) or non-ratable vided into two parts, as follows:
(inclusions are present but their length is below the 0.5 severity 13.3.1.1 The length of the longest inclusion shall be re-
limit or their width is < 2 µm), or their diameter is < 3 µm. corded first. It shall be supplemented to describe the inclusion
12.6.7 Information pertaining to the composition of the width by a superscript T for thin or H for heavy. A thin
inclusions (Types A to D) may be provided if desired. For rare inclusion is defined as being 10 µm (0.0004 in.) or less in width
earth- or calcium-treated steels, or other steels with nontradi- over more than 50 % of its entire length. Likewise, a heavy
tional deoxidation approaches, the chemical composition of the inclusion must have a thickness of 30 µm (0.012 in.) or more
inclusions, in general terms, must be reported with each rating. over the majority of its length. Inclusions greater than 10 µm
Microanalytical techniques may be required to obtain such but less than 30 µm wide shall not be represented by a T or H
information if the operator is not able to identify the inclusions superscript. Supercripts d (disconnected), vd (very discon-
by light optical examination. nected), and g (grouped) may also be used to describe the
12.6.8 Supplementary stereological data determined during degree of connectivity or clustering as illustrated in Fig. 8.
analysis may be included in the test report as desired. Stan-
13.3.1.2 The average length of all inclusions one unit and
dardization of such test data is not governed by this practice
longer in length, but excluding the longest inclusion, shall be
(see Practice E 1245).
reported as a single number, followed by a superscript denoting
13. Method B (Length) the number of inclusions averaged.
13.1 Introduction—This test method requires a survey of a 13.3.2 When required, a series of comparison photomicro-
160 mm2 polished surface area of the specimen at 1003. Any graphs at 1003, which illustrates all other nonmetallic par-
inclusion whose length is 0.127 mm or longer is to be ticles present, may be used to characterize the background
measured and individually tallied. appearance of the specimen. If used, these shall be labeled A,
13.2 Procedure: B, ... etc., in order of increasing inclusion population. The
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Image analysis software is then used to evaluate the inclusion 15.5.7 Use a previously written computer program to sepa-
content of the material. rate the inclusion images by type and thickness, then calculate
15.5 Image Analysis Procedure: severities based on length or number based on the rules listed
15.5.1 Place the specimen on the microscope stage so that in Section 12. The program should also store results, control
the specimen surface is perpendicular to the optical axis. With stage movements (if an automated stage is used), and generate
an inverted-type microscope, simply place the specimen face- the test report.
down on the stage plate and hold in place with the stage 15.5.8 If the width of an A inclusion, or a B or C stringer,
clamps. With an upright-type microscope, place the sample on varies and becomes less than 2 µm over part of its length,
a slide and level the surface using clay or plasticene and a detect as much of it as possible and calculate the severity based
hand-leveling press. Certain upright microscopes can be on the detected length. For specimens from wrought products
equipped with an autoleveling stage for mounted specimens. If with high degrees of reduction, where the majority of the
the sample must be leveled using clay, the tissue paper placed inclusions are < 2 µm thick, based on producer-purchaser
between the specimen surface and the leveling press ram may agreement, the minimum thickness of the thin series can be set
adhere to the surface and present artifacts for measurement. In
some cases, adherent tissue can be blown off the specimen
surface. An alternative procedure to avoid this problem is to 15
Forget, C., “Improved Method for E1122 Image Analysis Nonmetallic
place an aluminum or stainless steel ring form, which has been
Inclusion Ratings,” MiCon 90: Advances in Video Technology for Microstructural
flattened slightly in a vise to an oval shape, between the sample Control, ASTM STP 1094, American Society for Testing and Materials, Philadelphia,
and the ram. If the specimen was mounted, the ring form will 1991, pp. 135–150.
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Number. Therefore, if a B inclusion is oversized either in accurate Method D rating requires considerable effort.
length or thickness, that portion that is within the field 18.4 The accuracy of Method C ratings is significantly
boundaries shall be included in the appropriate Thin or Heavy influenced by misidentification of S Type (deformable oxide)
severity level measurement. Likewise, if an oversize D inclu- inclusions. When such problems are not encountered, steels
sion is encountered in a field, it also is included in the count with low inclusion contents will agree within 61 unit, while
that determines the D heavy rating. steels with high inclusion contents will agree within 62 units
16.3 Expression of Results: of severity. Method C, Plate II, is only used to rate oxides,
16.3.1 Results are expressed in terms of two rating numbers never sulfides.
reflecting B-type and D-heavy type inclusion contents. 18.5 The precision of ratings made by the use of Plate I-r
16.3.2 The number of B-type fields recorded at each sever- generally agrees with the chart severity increments used but
ity level times the severity level is summed (see Table 5) and may in certain cases be slightly higher. For very low inclusion
normalized by dividing by the total rated area, in square inches, content steels, automatic image analysis methods (as covered
of all samples. The nearest whole number is recorded as the by Practices E 1122 and E 1245) are preferable where ratings
rating. below the minimum rating (1⁄2) are possible. Note that micro-
16.3.3 The number of D units is summed (see Table 5) and scopic Methods A and D stipulate minimum sizes for ratable
normalized by dividing by the total rated area, in square inches, inclusions; thus a field or a specimen may contain inclusions
of all samples. The nearest whole number is recorded as the that are identifiable but not ratable because they are below the
rating. minimum size for a non-zero rating.
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