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MEASURING INCLUSION CONTENT BY ASTM E 1245

George F. Vander Voort


Consultant – Struers Inc.

ABSTRACT

Over the past forty-plus years, steelmakers have introduced improved practices for reducing the
inclusion content of steels. The success of these practice changes can be monitored in a variety of
ways. Chemical analysis of the bulk sulfur and oxygen contents provides a relatively simple means to
assess the impact of these changes. However, microscopical test methods are still needed to assess
the nature of the inclusions present. Traditional chart-based measurement methods have wide
acceptability, and their data are well understood by both purchaser and producer for heat acceptance
purposes. These methods do have inherent weaknesses which limit their usefulness for quality
control and database applications. Image analysis-based chart measurements are an improvement
over manually generated chart ratings, but the data still does not lend itself to databases and
statistical comparisons. ASTM Committee E-4 on Metallography has developed a stereologically-
based image analysis standard test method, E 1245, which provides the necessary data in a form
which is easily databased and analyzed statistically. The presentation will describe E 1245 and show
how data from different heats and melting practices can be compared statistically to ascertain valid
test differences.

Introduction

The comparison chart method has been the traditional approach for rating the inclusion content of
steels. The ASTM E45 (1) and ISO 4967 (2) chart methods as well as several other national
standards are based on the original Swedish JK Chart methods (3). A somewhat different chart
method (4) is used in Germany as VDEh 1570 or DIN 50602. While chart methods have been used
for more than eighty years and are still widely used, they do suffer from a number of problems (5, 6).
Steelmaking practices have changed over the years with considerable diversity in deoxidization
practice which influences the nature of the inclusion population. The original charts, developed using
acid open-hearth steel, do not adequately reflect the appearance of inclusions in today’s steels. (The
current E45 charts were computer generated). The chart picture images, relative to the severity
values, were inaccurate. (The ASTM E45 charts have been modified to addresses this problem.)
Numerous inter-laboratory rating studies have shown that inclusion chart ratings suffer from poor
repeatability and reproducibility (6). Chart data has a limited number of severity values thus limiting
sensitivity and ability to discriminate between heats. The worst field method is easiest to perform but
is qualitative at best, while the quantitative method (every field within a fixed area is rated) is very
tedious, and the data are very cumbersome to handle. In either case, the qualitative or quantitative
methods, the data are ill-suited for use in spreadsheet-type databases.
Recognizing these problems, many people have tried to develop modified chart methods or alternate
counting/measurement schemes (5). None of these have been adapted by industry. There are two
major obstacles to the adoption of a new inclusion rating system. First, the steel purchaser or
designer has no familiarity with the data produced by the new method, so they do not know what
acceptance limits should be specified. Secondly, the steelmaker also has no familiarity with data from
the new system, so they do not know if they can meet the specified limits. Only by rating numerous
heats of steel by the chart method and the new method, with the data openly published, can this
problem be resolved.
Consequently, the writer decided to try to improve the chart method by using automatic image
analysis (7) and wrote ASTM E1122, adopted initially in 1986 (8). E1122 was incorporated within
E45 in 2006 and then withdrawn. However, to address some of the other problems such as the
redefinition of the inclusion measurement values for specific severity levels, other changes (9) to both
E1122 and E45 were proposed, balloted, and adopted.
Over the years, many people have used stereological procedures (5), chiefly point-counting to define
the inclusion volume fraction, to determine the inclusion content. When image analyzers became
more powerful and more common in the laboratory in the 1980s, the writer prepared ASTM E1245
(10) which was adopted in 1988. As computer power has increased, E1245 has been modified. The
original method used field measurements exclusively, while the current version combines field
measurements and feature-specific measurements. A few examples of the nature and use of E1245
data have been published (11 - 13).
In this method, oxides and sulfides are separated by gray level differences, and the following
measurements are made separately for sulfides and oxides in each specimen.
 Area fraction (estimate of the volume fraction) usually expressed as a percentage, AA.
 Number of inclusions per unit area (mm2), NA
 Average inclusion length (m), L
 Average inclusion area (m2), A
 Mean free path, the mean edge-to-edge spacing between all inclusions in the through-
thickness direction (m),  or MFP
The mean free path is not a nearest neighbor spacing. It is calculated according to:
 = 1 - AA
NL
where the area fraction is a fraction (not a percentage), and N L is the number of interceptions of
inclusions with lines parallel to the through thickness direction. On older image analyzers, the scan
lines were used, but on current image analyzers the frame grabber rows are used. However, because
of the nature of this equation,  cannot be calculated for each field if any are inclusion free. Hence,
except for sulfides in free-machining steels,  is normally calculated only after a number of fields are
measured; i.e., at the end of the analysis run. Today, a “panoramic” image analysis approach can be
taken which eliminates this restriction. Otherwise, AA and NA are field measurements, and the mean
and standard deviation of the  measurements are calculated after the analysis run. L and A are
based on the mean of the individual inclusion measurements rather than a mean of the mean length or
mean area per field. Consequently for each analysis run, the mean and standard deviations of A A, NA,
L, and A are determined, but only a mean  value is determined unless the panoramic method is used.
If there are no blank fields,  can be calculated for each field, and the mean and standard deviation
could be calculated for that analysis run.
If each specimen in the heat lot is evaluated using E 1245, then the mean values for each specimen
can be used to calculate the heat mean and standard deviation for each measurement type. This
brings up a practical mathematical problem. Strictly speaking, as the area fraction drops below 2%,
the distribution of any field measurement deviates from a Gaussian distribution, and it is not valid to
calculate an arithmetic standard deviation. However, correcting this problem is so difficult that
arithmetic standard deviations are still calculated. However, the distribution of specimen averages
for a larger number of specimens from a heat lot is Gaussian. Consequently, the arithmetic standard
deviation of specimen mean values is valid. This is good as many times we want to compare data for
different heats of steel, and we need the heat mean and standard deviation (plus the number of
specimens measured).
The purpose of this paper is to compare chart ratings made by ASTM E45/E1122 with stereological
E1245 data. The tested bearing steels were made by different manufacturers using a variety of
steelmaking procedures. Hence, we can also evaluate the effect of different melting practices upon
the inclusion content.

RESULTS
Test Material
For this study, longitudinally-oriented surfaces were prepared from the mid-thickness location of
billets and bars of a variety of heats of 52100 bearing steel. In most cases, the specimens came from
the usual top, middle, and bottom locations with respect to the cast ingot, but in a few cases they
came from opposite ends of randomly selected bars.
Electric furnace steel came from three sources. Source 1 provided test material from three heats
produced within a short time frame - heats 1a, 1b, and 1c. These electric furnace heats were ladle
treated, vacuum degassed, and bottom poured. Source 2 provided material from one heat that was
electric furnace melted, ladle treated, vacuum-degassed and continuously cast - heat 2. Source 3
provided material from two heats that were electric furnace melted, ladle treated, and bottom poured
- 3a and 3b.
The next material heat, ESR-4, was electric furnace melted and then electroslag remelted. These
samples were taken from adjacent locations from the same bar. This steel was processed around
1980 and was used in an earlier inter-laboratory manual rating study. It may not be representative of
today’s ESR technology.
Samples from a production double vacuum melt VIM/VAR heat (vacuum induction melt, vacuum arc
remelt) and one 500 lb. laboratory VIM/VAR heat were tested, PV-5 and LV-6, respectively. Hence,
these heats cover the range of 52100 used in bearing steels today.

Measurements
The specimens were polished on longitudinal cross-sections after hardening the specimens (to
provide optimum inclusion retention). Automatic polishing equipment was used starting with a
coarse grit SiC paper to remove cutting damage and make the surfaces of the specimens co-planar.
Next, they were ground using 15 m diamond slurry on a heavy nylon cloth. Then, they were
polished using 3m diamond on a DP-Pan cloth followed by final polishing using colloidal silica on
an MD-Floc polishing cloth.
Image analysis measurements were performed using 200 randomly selected fields per specimen for
ASTM E1245 while 160 mm2 surface area was evaluated per ASM E1122. Table 2 lists the heat
averages for the JK data based on the averages of the worst field ratings for all of the specimens in
each heat. One problem with worst field ratings is immediately apparent but only if the number of
worst fields per specimen is known to the reader. Note that six of the nine heats have ratings for C-
type inclusions of both thicknesses. However, each specimen had only a few such fields with C
ratings. Such ratings generally arise in these heats when B-type oxides are touching so that their net
length meets the C requirement. Manual raters should call these B inclusions despite their
continuous nature. The primary weakness of the JK data shown in Table 2 is that it is not
quantitative. It only shows what the rating of the worst field was. It is difficult to use this data to
clearly discriminate between heats.
The E1245 oxide and sulfide measurement data are given in Tables 3 and 4. Bear in mind that the
standard deviations and number of specimens for each value are also known but not reported here.
The oxide data is more informative for comparing the heats as the aim sulfur contents of these heats
may be quite different; that is, while the steelmaker always wants the lowest possible oxygen content,
that may not be the case for the sulfur content. However, the sulfide data is provided for comparison
with the JK A-type (sulfide) ratings.
Table 5 shows the heats ordered by area fraction of sulfide inclusions and the corresponding JK
ratings for the A-type (sulfide) inclusions. In general, there is a reasonable correlation between the
JK ratings considering both the thin and thick ratings and the sulfide area fractions. The major
exception is heat EF-2 where the JK ratings were much lower than would be expected. Further,
PV-5 and LV-6 had essentially identical area fractions, but the A-thin ratings differed significantly.
Table 6 shows the heats ordered by area fraction of oxide inclusion and the corresponding JK ratings
for the B- and D-type inclusions. The C-type inclusions were not included for the reason noted
above. Considering only the thin ratings, there is general agreement that the first three heats listed
had the highest oxide content while the last two heats had the lowest oxide inclusion content. In
between, the agreement is not as good. The heavy ratings are more erratic than the thin ratings. One
could conclude that worst field JK ratings are suitable for discriminating between heats with
substantial differences in inclusion content and perhaps less than adequate for separating heats with
small differences in the inclusion content.
The inclusion ratings suggest that, of the electric furnace heats, the new EF-1 heats were similar to
the EF-2 heat and both had lower inclusion contents than the two EF-3 heats. The E1245 data can
be used to compare these heats. A few examples of such comparisons will be presented to illustrate
the value of true quantitative data.
Table 7 repeats the E1245 oxide data for the three EF-1 heats and EF-3b. The T-test was used to
determine if the difference between the means is statistically significant. For example, Table 7 shows
that the oxide area fraction of heat EF-3b is higher than that of the three EF-1 heats and that these
differences were significant at the 99% confidence level. On the other hand, the analysis showed that
there was not statistical difference among any of the area values. The mean free path comparison
reveals an interesting fact. Note that the MFP value of EF-1a was the largest, yet the statistical
significance of the difference between the MFP of EF-1a and EF-3b was lower than that of the other
two heats relative to that of EF-3b. At first glance, this seems to be wrong. However, the standard
deviation of the MFP of EF-1a was six times greater than that of EF-1b and EF-1c which accounts
for the lower confidence level.
Table 8 compares the oxide measurements for EF-2, which was an electric furnace, ladle treated,
vacuum degassed and continuously cast heat versus EF-3a and 3b, which were electric furnace
melted, ladle treated and bottom poured, but were not vacuum degassed. Consequently, the volume
fraction and number per unit area for the degassed EF-2 specimens were significantly lower while the
mean free path was significantly greater than the non-vacuum degassed heat EF-3. The size
differences were not significant.
Table 9 compares the oxide data for EF-2 with that of the production VIM/VAR heat, PV-5. In like
manner, the VIM/VAR heat had a significantly lower oxide volume fraction and number per unit area
of particles while the mean free path was significantly greater. Again, there was no significant
difference in the lengths or areas of the oxides. Table 10 compares the oxides in EF-1a, 1b and 1c, a
heat that was melted in the electric furnace, ladle treated, vacuum degassed and bottom poured, with
the specimens from the 500 lb. laboratory VIM/VAR heat, LV-6. Not surprisingly, all of the oxide
measurements for the LV-6 heat specimens were significantly better than the EF-1 heat specimens.
Table 11 shows a comparison of the oxide measurements in electric furnace heats EF-3a and EF-3b
and VIM/VAR heat PV-5. Here the area fraction, number per unit area, and mean free path values
for the production VIM/VAR heat are clearly lower than the corresponding values for the EF heats,
and the differences are strongly significant. However, in the N A values, we again see an apparent
discrepancy. The difference between PV-5 (1.2) and EF-3a (7.0) is less significant than the difference
between PV-5 and EF-3b (3.3). The reason for this apparent anomaly again lies with the standard
deviations, that of EF-3a is more than 8 times larger than that of EF-3b (and 10 times larger than that
of PV-5). Note that the differences between the L and A values are not statistically significant. This
is true even for the area values where there appears to be an obvious difference. Again, these
differences are not statistically significant due to the magnitude of the standard deviations.
Table 12 lists the data for the EF-3a and 3b specimens, the electric furnace heat that was ladle treated
and bottom poured, but was not vacuum degassed, compared to the data for the specimens from the
500 lb. laboratory VIM/VAR heat, LV-6. Again, all the results for the LV-6 heat were statistically
better that the EF-3b specimen but compared to the EF-3a specimen. The area measurement
difference showed no statistical significance. But, all of the other data for the LV-6 specimens were
statistically better than the data for the EF-3a specimens.
Finally, Table 13 shows a comparison of the data between the production VIM/VAR heat, PV-5,
versus the laboratory VIM/VAR heat, LV-6. The differences were weaker than for the other
comparisons. But, the laboratory VIM/VAR heat had a significantly lower volume fraction of oxides
and their length and area were significantly smaller but their number per unit area and mean free path
were not significantly different.

Conclusions
Chart ratings of inclusions have limited value and have been shown in interlaboratory test programs
to be non-reproducible between raters and prone to mis-classification problems, even for experienced
raters. Today, performing E45 ratings by image analysis does yield better reproducibility. But, the
data is not statistical and it is difficult to compare heats made by the same or by different melting
practices. The E1245 method has the advantage of being performed using stereological type
measurements, although only one plane is evaluated. But, the data per specimen and per heat is
quantitative and can be compared mathematically to determine if one process is better or worse than
another. Heat data can be collected into spreadsheets to follow melting practice changes and results.
But, the problem now exists that despite the publication of results using E1245, purchasers are still
largely unaware of the method and have not created purchase requirements using the method, except
for a few products. That is needed to get the standard implemented commercially, as opposed to
being mainly a research tool.

References
1) ASTM E45: Standard Test Methods for Determining the Inclusion Content of Steel.
2) ISO 4967: Steel-Determination of Content of Non-metallic Inclusions - Micrographic Method
Using Standard Diagrams.
3) B. Rinman, et al., “Chart for the Estimation of Inclusion in Steel,” Jernkontoret Annal., Vol.
120, 1936, pp. 199 - 226.
4) Barteld, K. and A. Stanz, “Microscopic Examination of Specialty Steels for Non-metallic
Inclusion with Reference Inclusion Charts,” Archiv für das Eisenhuettenwesen, Vol. 42,
August 1973, pp. 581 - 597.
5) Vander Voort, G. F., “Inclusion Measurement,” Metallography as a Quality Control Tool,
Plenum Press, NY, 1980, pp. 1 - 88.
6) Vander Voort, G. F., “Difficulties Using Standard Chart Methods for Rating Nonmetallic
Inclusions,” Industrial Heating, Vol. 84, No. 1, January 2016, pp. 34-37.
7) Vander Voort, G. F., and F. Golden, “Automating the JK Inclusion Analysis,” Microstructural
Science, Vol. 10, 1982, pp. 277 - 290.
8) ASTM E1122: Standard Practice for Obtaining JK Inclusion Ratings Using Automatic Image
Analysis.
9) Vander Voort, G. F., and R. K. Wilson, “Nonmetallic Inclusions and ASM Committee E-4”,
ASTM Standardization News, Vol. 19, May 1991, pp. 28 - 37.
10) ASTM E1245: Standard Practice for Determining the Inclusion or Second-Phase Constituent
Content of Metals by Automatic Image Analysis.
11) Vander Voort, G. F., “Measurement of Extremely Low Inclusions Contents by Image Analysis”,
ASTM STP987: Effect of Steel Manufacturing Processes on the Quality of Bearing Steels,
ASTM, Philadelphia 1988, pp. 226 - 249.
12) Vander Voort, G. F., “Characterization of Inclusions in a Laboratory Heat of A1S1 303 Stainless
Steel,” Inclusions and Their Influences on Material Behavior, ASM International, 1988, pp.
49 - 64.
13) Vander Voort, G. F., “Computer-aided Microstructural Analysis of Specialty Steels,” Materials
Characterization, Vol. 27, No. 4, December 1991, pp. 241 - 260.
Table 1: Test Material Studied
Melting Process Heat Codes
EF-LT-VD-BP EF-1a, 1b and 1c
EF-LT-VD-CC EF-2
EF-LT-BP EF-3a and 3b
EF-ESR (1980 vintage) ESR-4
Production VIM/VAR (20,000 lbs.) PV-5
Laboratory VIM-VAR (500 lbs.) LV-6a and 6b

Table 2: Heat Averages for E45/E1122 Data

A Type B Type C Type D Type


Code Thin Thick Thin Thick Thin Thick Thin Thick
EF-1a 0.86 0.67 1.17 0 0.58 0.53 0.92 0.39
EF-1b 0.94 0.56 1.11 0.96 0.58 0.42 0.94 0.33
EF-1c 0.92 0.69 1.00 0.03 0.36 0.39 0.96 0.25
EF-2 0.50 0.30 0.50 0.20 0 0 1.00 0.05
EF-3a 0.92 0.83 1.67 0.50 0.33 0.58 1.08 0.50
EF-3b 1.08 0.75 1.67 0.58 0.67 0.75 1.17 0.50
ESR-4 0.50 0.5 1.50 0 0.25 0.13 1.00 0.25
PV-5 0.20 0 0.25 0.05 0 0 0.60 0.05
LV-6 0.08 0 0.08 0.17 0 0 0.75 0.08
Table 3. Heat Averages for Oxides by E1245
Heat AA NA L A MFP
Code (%) (mm-2) (m) (m2) (m)
EF-1a 0.0039 2.0 7.2 28.5 173147
EF-1b 0.0038 1.6 8.1 37.6 119992
EF-1c 0.0051 2.5 7.2 28.7 92186
EF-2 0.0039 2.2 6.6 28.3 105844
EF-3a 0.0109 7.0 6.8 27.6 41812
EF-3b 0.0095 3.3 8.6 31.1 40482
ESR-4 0.0065 2.7 7.7 34.4 56039
PV-5 0.0013 1.2 7.3 43.5 283047
LV-6 0.0005 1.1 4.4 16.1 373430

Table 4: Heat Averages for Sulfides by E1245


Heat Code AA NA L A MFP
(%) (mm-2) (m) (m2) (m)
EF-1a 0.026 17.7 6.9 17.0 10713
EF-1b 0.029 16.7 7.3 19.5 9922
EF-1c 0.039 20.9 8.3 20.9 6811
EF-2 0.046 40.4 6.1 12.3 5007
EF-3a 0.056 28.5 7.4 24.0 6010
EF-3b 0.050 17.8 8.9 30.3 7280
ESR-4 0.018 19.0 4.4 11.0 16351
PV-5 0.007 11.3 4.1 9.1 40720
LV-6 0.008 21.1 2.7 4.3 27731
Table 5. Ranking by Sulfide Area Fraction
Specimen AA A
Code (%)
Thin Heavy
EF-3a 0.056 0.92 0.83
EF-3b 0.050 1.08 0.75
EF-2 0.046 0.50 0.30
EF-1c 0.039 0.92 0.69
EF-1b 0.029 0.94 0.56
EF-1a 0.026 0.86 0.67
ESR-4 0.018 0.50 0.25
LV-6 0.008 0.08 0

Table 6. Ranking by Oxide Area Fraction


Specimen AA B D
Code (%) Thin Heavy Code (%)
EF-3a 0.0109 1.67 0.50 1.08 0.50
EF-3b 0.0095 1.67 0.58 1.17 0.50
ESR-4 0.0065 1.50 0 1.00 0.25
EF-1c 0.0051` 1.00 0.03 0.86 0.25
EF-1a 0.0039 1.17 0. 0.92 0.39
EF-2 0.0039 0.50 0.20 1.00 0.05
EF-1b 0.0039 1.11 0.06 0.94 0.33
PV-5 0.0013 0.25 0.05 0.60 0.05

Table 7: Comparison of Oxides: EF Heat 1a, b, and c versus Heat 3a and 3b


Heat AA NA L A MFP
Code (%) (mm-2) (m) 2
(m ) (m)
EF-1a 0.0039 2.0 7.2 28.5 173147
EF-1b 0.0038 1.6 8.1 37.6 119992
EF-1c 0.0051 2.5 7.2 28.7 92186
EF-3a 0.0109 7.0 6.8 27.6 41812
EF-3b 0.0095 3.3 8.6 31.1 40482

Statistical Significance, Confidence Level (t-test)


EF-1a vs. 3a 99% 90% nss nss 90%
EF-1b vs. 3a 99% 95% nss nss 99%
EF-1c vs. 3a 98% 90% nss nss 99%

EF-1a vs. EF-3b 99% 99% 95% nss 90%


EF-1b vs. EF-3b 99% 99% nss nss 99%
EF-1c vs. EF-3b 99% 90% 95% nss 99%
nss = Difference Is Not Statistically Significant

Table 8: Comparison of Oxides: EF Heat 2 vs. EF Heats 3a and 3b


Heat AA NA L A MFP
Code (%) (mm-2) (m) (m2) (m)
EF-2 0.0039 2.2 6.6 28.3 105844
EF-3a 0.0109 7.0 6.8 27.6 41812
EF-3b 0.0095 3.3 8.6 31.1 40482

Statistical Significance, Confidence Level (t-test)


EF-2 vs. 3a 98% 90% nss nss 98%
EF-2 vs. 3b 99% 90% 95% nss 99%

Table 9: Comparison of Oxides: EF-2 vs. PV-5


Heat AA NA L A MFP
Code (%) (mm-2) (m) (m2) (m)
EF-2 0.0039 2.2 6.6 28.3 105844
PV-5 0.0013 1.2 7.3 43.5 283047

Statistical Significance, Confidence Level (t-test)


EF-2 vs. PV-5 99% 90% nss nss 99%

Table 10: Comparison of Oxides: EF-1a, 1b and 1c vs. LV-6


Heat AA NA L A MFP
Code (%) (mm-2) (m) (m2) (m)
EF-1a 0.0039 2.0 7.2 28.5 173147
EF-1b 0.0038 1.6 8.1 37.6 119992
EF-1c 0.0051 2.5 7.2 28.7 92186
LV-6 0.0005 1.1 4.4 16.1 373430

Statistical Significance, Confidence Level (t-test)


EF-1a vs. LV-6 99% 99% 99% 90% 95%
EF-1b vs. LV-6 99% 98% 99% 99% 99%
EF-1c vs. LV-6 99% 99% 99% 90% 99%

Table 11: Comparison of Oxides: EF Heats 3a and 3b vs. Heat PV-5


Heat AA NA L A MFP
Code (%) (mm-2) (m) (m2) (m)
EF-3a 0.0109 7.0 6.8 27.6 41812
EF-3b 0.0095 3.3 8.6 31.1 40482
PV-5 0.0013 1.2 7.3 43.5 283047

Statistical Significance, Confidence Level (t-test)


EF-3a vs. PV-5 99% 95% nss nss 99%
EF-3b vs. PV-5 99% 99% nss nss 99%
Table 12: Comparison of Oxides: EF Heats 3a and 3b vs. Heat LV-6
Heat AA NA L A MFP
-2
Code (%) (mm ) (m) (m2) (m)
EF-3a 0.0109 7.0 6.8 27.6 41812
EF-3b 0.0095 3.3 8.6 31.1 40482
LV-6 0.0005 1.1 4.4 16.1 373430

Statistical Significance, Confidence Level (t-test)


EF-3a vs. LV-6 99% 95% 80% nss 99%
EF-3b vs. LV-6 99% 99% 99% 90% 99%

Table 13: Comparison of Oxides: Vim/VAR Heats PV-5 vs. Heat LV-6
Heat AA NA L A MFP
-2
Code (%) (mm ) (m) (m )2
(m)
PV-5 0.0013 1.2 7.3 43.5 283047
LV-6 0.0005 1.1 4.4 16.1 373430

Statistical Significance, Confidence Level (t-test)


PV-5 vs. LV-6 90% nss 98% 90% nss

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