MATERIALS

MATERIALSCHARACTERIZATION
CHARACTERIZATION
& TESTING
& TESTING

Difficulties Using Standard

Chart Methods for Rating
Nonmetallic Inclusions
George F. Vander Voort Vander Voort Consulting; Wadsworth, Ill.
Checking our incoming raw-material quality often involves rating nonmetallic inclusions,
particularly when heat treating to high hardnesses. We want to know that the steel we are heat
treating is clean. Learn why obtaining consistent results is a challenge for more than one reason.

ver the years, ASTM Committee E-4 on Metallography

has conducted interlaboratory test programs to evaluate
the precision and bias associated with measurements
of microstructure using proposed and existing test
methods. ASTM decided in the late 1970s that all test methods
that generated numerical data must have a precision and bias
section defining the repeatability and reproducibility of the
method.
Defining bias associated with a test method is difficult
unless there is an absolute known value for the quantity being
measured, and this is not possible when microstructural
features are being measured. This paper shows the results for
an interlaboratory test using Method A, worst-field ratings
of inclusions in steels by ASTM E-45. The results from nine
people who were reported to be qualified, regular users of
the method revealed consistent problems of inclusion-type
misclassification and a wide range of severity ratings for each
specimen.

Introduction
Created in 1942, ASTM E45 was based on an earlier[1,2]
chart developed by Jernkontoret in Sweden. The charts were
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JANUARY 2016 IndustrialHeating.com

designed to determine the size, distribution, number and types

of indigenous inclusions (naturally occurring particles that form
before or during solidification due to limited solid solubility for O
and S) in steels.
Originally, E45 included three charts Plates I, II and III

20m

Fig. 1. Example of manganese sulfides in a lightly resulfurized alloy steel

(blue arrows) and a globular aluminate (red arrow); longitudinal plane.

100m

50m

Fig. 2. Examples of manganese silicates in a non-aluminum killed alloy

steel (longitudinal plane).

but now there are two, Plates 1r and II. Plate 1r replaced Plates
I and III after these charts were measured[3] and corrected in
the creating of the image-analysis method for making E45 JK
inclusion ratings,[4,5] which was published as E1122 in 1992 and
incorporated into E45 in 2006.
The JK chart the original Plate I categorized indigenous
inclusions as sulfides (type A), aluminates (type B), silicates (type
C) and globular oxides (type D), although the classification was
stated to be only by morphology. There were thin and thick
categories of each based on their thickness (or diameter for the
D types), and the severity ratings varied in whole increments
from 1 to 5. Plate III was similar, but the severity limits were in
0.5 increments from 0.5-2.5.

Inclusion Rating Challenges

Basing the categorization of A and C types on morphology
alone creates inherent confusion in ratings because both
elongated, malleable inclusion types look similar. The charts
do not show the gray-level difference between gray sulfides and
darker, blackish, glassy-looking silicates. Some raters seem to
regularly confuse the two types. Obviously, sulfides and silicates
have markedly different effects on steel products.
Similar charts for rating inclusions have been developed by
numerous countries and companies over the years and by ISO.[3]
At least two such charts depict sulfides as being lighter than
silicates. The tips of sulfides also appear to be more rounded
than silicates, which appear to be sharper, but these differences
may be difficult to see at the usual depiction of the inclusions at
100X magnification by the chart pictures.
These chart ratings were all done qualitatively until E1122
was developed, which utilized an image analyzer to make the

Fig. 3 Example of a gross aluminate stringer in P20 mold steel

(longitudinal plane).

ratings. The operator scans a specific-sized area on a polished

specimen and then records the worst ratings of each inclusion
type and thickness observed (Method A). Alternatively, the
operator can scan the area field by field and record the ratings of
the inclusions in every field (Method D). Method A, of course,
takes far less time to perform manually than Method D and is
more commonly utilized. By image analysis, there is no realtime difference between performing Methods A and D.
The success of such ratings manually in defining the inclusion
content in a heat of steel hinges upon a number of factors:
Relevance of the billet test locations and test-plane
orientation in defining the total inclusion content and the
distribution of the inclusions relative to the ingot location or
concast billet location
Quality of the specimen preparation
Grading of the inclusion dimensions by the chart and the
relevance of the deformation pictured to the degree of hot
reduction of the billets
Similarity of the inclusion morphologies depicted in the
chart pictures to those in the steel being evaluated
Validity of the rating method
Statistical value of the chart ratings
Correlation of the chart ratings to other methods for
assessing the inclusion content
While manual chart ratings are relatively simple to
perform and the analysis time is reasonably fast, they do
suffer from numerous disadvantages that substantially
degrade the reliability, reproducibility and repeatability of the
measurements. The E45 charts were developed based upon
the effect of hot-working deformation on the inclusion length,
or stringer length, going from ingot to a 4- x 4-inch billet
size. Naturally, this degree of deformation is not obtained in a
casting or in a large forging and will be greater for plate, bar,
sheet or strip products.
IndustrialHeating.com JANUARY 2016

35

MATERIALS CHARACTERIZATION
& TESTING

Round-Robin Interlaboratory
Test Program Results
The writer organized a round robin using specimens cut
sequentially along billets of three steels with varying sulfur
content and melting practices, some of which were Al-killed
and some that were not. Nine different people analyzed the
specimens using Method A (worst field) of ASTM E45. The
data is summarized in Tables 1-3. The specimen used for the
data in Table 1 was type S7 tool steel, which is not Al-killed
and does exhibit very classic silicate inclusions of the C type.
Its oxygen content is a bit on the high side for a 0.50% carbon
tool steel (electric furnace, non-degassed). Its sulfur content is
relatively normal for tool steels.
Note the wide range of severity values for all inclusion
types, indicating imprecision and insensitivity in the ratings.
S7 definitely has silicates but should have virtually no oxide
stringers of the B type, but the B thin and B thick ratings ran
from severities of 0 to 3 and 0 to 2.5, respectively, with averages
of 0.78 and 0.89.
Meanwhile, some raters did not rate any oxides as C types,
although they predominate in S7. No doubt, they rated the
silicates as type A sulfides. There will be a few isolated oxides
that are not elongated enough to be classified as stringers
and can be rated as D types. The A ratings are a bit high for
a steel with 0.017% S (compare these A ratings to that of the
resulfurized steel in Table 2).
Table 1. AISI S7 (0.017% S, <0.005% Al and 95 ppm O)
rated by 9 metallographers
E45
method A

A
thin

A
thick

B
thin

B
thick

C
thin

C
thick

D
thin

D
thick

Range

1-4

1-3

0-3

0-2.5

0-4

0-5

1-2

0-2

Mean

2.33

2.0

0.78

0.89

2.89

3.0

1.22

0.72

0.83

0.71

1.09

1.14

1.24

1.39

0.44

0.67

95% CL

0.68

0.58

0.89

0.93

1.01

1.13

0.36

0.55

29

28.9

114

104

35

38

29

76

% RA

Table 2 shows E45, Method A ratings for a resulfurized

41S50 alloy steel at 0.065% S (3.8 times the sulfur content of the
S7 specimens shown in Table 1). Unlike the S7 heat, the 41S50
was Al-killed and its oxygen content is a bit lower. Despite the
much greater S content, the A-type sulfide ratings are not much
different than for the S7 tool steel.
The A thin and A thick ratings both varied from 0 to 4,
versus 1-4 (thin) and 1-3 (thick) for the S7 specimen with onequarter as much sulfur. The averages for the nine A thin and
thick ratings were 2.33 and 2.0 for the S7 steel with 0.017% S
and 2.78 and 1.72 for the 41S50 specimens with 3.8 times as
much sulfur. The 41S50 specimen should have B-type aluminate
stringers present, but no C-type elongated silicates. However,
the C thin and thick ratings for the 41S50 specimens varied
from 0 to 5 and 0 to 4, with mean values of 2.0 and 0.89. These
C ratings must actually be for A-type sulfides. Note that the
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JANUARY 2016 IndustrialHeating.com

% relative accuracy values for the 41S50 ratings are noticeably

higher than for the S7 ratings.
Table 3 shows E45 Method A ratings for 52100 bearing steel
made in the electric furnace, vacuum degassed with electrodes
then remelted by the electroslag remelting (ESR) process. ESR
produces a very low sulfur content; 0.003% is barely above the
solubility level of sulfur in Fe, so there should be no type-A
sulfides at or above the 0.5 severity level. There were A thin and
thick ratings from 0.5 to 1.5 and 0 to 1.0, however, with mean
values of 1.12 and 0.5 respectively.
The oxide content should be very low, with an oxygen content
of 37 ppm. Since 0.020% Al was present, it would be unlikely to
see type-C silicates in these specimens. Also, with the very low
sulfur level and the higher-than-expected A ratings, it is hard to
envision sulfides being rated as silicates in these specimens.
Overall, the inclusion ratings are much lower than for the S7
and 41S50 specimens. Based upon my experience, however, the
EF-ESR 52100 inclusion ratings seem to be excessively high.
As would be expected, the standard deviations, 95% confidence
limits and % relative accuracy values for the EF-ESR 52100,
due to its lower S and O contents, are much lower (statistically
better) than the data for the S7 and 41S50 specimens.
Table 2. 41S50 (0.065% S, 0.057% Al and 68 ppm O)
rated by nine metallographers
E45
method A

A
thin

A
thick

B
thin

B
thick

C
thin

C
thick

D
thin

D
thick

Range

0-4

0-4

0-3

0-3

0-5

0-4

0-4

0-2

Mean

2.78

1.72

1.72

0.67

2.0

0.89

1.56

0.61

1.39

1.68

1.15

1.12

2.4

1.54

1.13

0.7

95% CL

1.13

1.37

0.94

0.91

1.96

1.26

0.92

0.57

% RA

40.8

80

54.5

136

98

141

59

93.6

Table 3. EF-ESR 52100 bearing steel (0.003 % S, 0.020% Al

and 37 ppm O) rated by nine metallographers
E45
method A

A
thin

A
thick

B
thin

Range

0.5-1.5

0-1

Mean

1.12

0.5

0.35

0.38

95% CL

0.31

0.34

% RA

27.8

68

30.6

B
thick

0.5-2.5 0.5-1.5

C
thin

C
thick

D
thin

D
thick

0-1

0-1

0-2

0-1

1.06

0.5

0.25

1.25

0.88

0.6

0.42

0.46

0.38

0.6

0.35

0.54

0.38

0.41

0.34

0.54

0.31

35.4

82.2

136

43

36

1.75

Conclusions
The data from this round robin (which is in agreement with
previous studies) clearly shows that ASTM E45 chart ratings
are neither precise nor reproducible. Repeatability was not
evaluated in this study.
The overall problem stems from a number of factors, as listed
above, which make chart ratings undependable. Yes, they are
fast and simple to do, but they are subjective. ASTM E1122
was developed to permit use of image analysis to perform E45

ratings. This method is much more precise and reproducible because inclusions in every
field are rated using the exact same criteria as defined in the standard. Even with better
image-analysis-generated E45 ratings, however, the value of the data in predicting the
performance of components in the field is still dubious.
A far better approach is to use stereologically based measurements of the oxides and
sulfides by ASTM E1245. The weakness here is that purchasers do not know what

All the best of

IndustrialHeating.com

content, all the time.

limits to use in purchase specifications.

To date, only one commercial product
standard[6] is known to this writer using
E1245 data for acceptance or rejection.
This problem could be alleviated
if image-analysis software produced
E1245 measurements simultaneously
when doing E45 chart ratings. Then
the purchaser would start to understand
the valuable nature of stereologically
based measurements of the area fraction,
number of inclusions per square mm
area, average length and cross-sectional
area, and spacing of oxides and sulfides
using E1245 with mean values and
standard deviations of the measurements
for data-basing test results.
The mean data values for all
specimens from a heat can be averaged
and standard deviations calculated.
Then differences between heats or
variations between melting practices or
vendors can be validly determined via
simple statistical procedures, such as the
student-t test.
For more information: Contact George F.
Vander Voort Vander Voort Consulting
LLC in Wasworth, Ill.; tel: 847-623-7648;
e-mail: georgevandervoort@hotmail.com;
web: www.georgevandervoort.com

References

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1. B. Rinman et al., Inclusion Chart for the

Estimation of Slag Inclusions in Steel,
Jernkontoret, Stockholm, Sweden, Uppsala
(1936), 24 pages
2. B. Rinman et al., Chart for the Estimation
of Inclusions in Steel, Jernkontoret Ann.,
Vol. 120, 1936, pp. 199-226
3. Inclusion Measurement, Metallography as
a Quality Control Tool, Plenum Press, NY,
1980, pp. 1-88
4. G. F. Vander Voort and J. F. Golden,
Automating the JK Inclusion Analysis,
Microstructural Science, Vol. 10, Elsevier
Science Publishing Co., NY, 1982, pp.
277-290
5. C. Forget, Improved Method for E1122
Image Analysis Nonmetallic Inclusion
Ratings, Micon 90: Advances in Video
Technology for Microstructural Control,
ASTM STP 1094, ASTM, Philadelphia,
1991, pp. 135-150
6. AAR Specification M-107/M-208, Rev.
2009, Wheels, Carbon Steel

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