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Progress in metallographic tests standards

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 Test standards are continually fine tuned
as knowledge of the subject and experience
with test methods are gained.
George F. Vander Voort *
Carpenter Technology Corp.
Reading, Pa.
aterials specifications are a neces-
M sary part of commerce, and are used
by manufacturers, purchasers, and
consumers. Thousands of specifi-
cations, covering a wide range of requirements
including chemical composition, mechanical and
physical properties, microstructure, dimensions,
and appearance have been written by pur-
chasers, government agencies, and national and
international technical societies. It also is
necessary to have specifications that describe
how these characteristics/properties are to be
measured . These are called standard test
methods if their purpose is to produce numerical
data. One general category of such methods is
metallographic-test methods, which have been
developed by many organizations. However, the
most widely used are those developed by
American Society for Testing and Materials
(ASTM) Committee E-4 on Metallography.
What started as a two-page document in 1916
covering macroscopic and microscopic metal-
lographic procedures, has evolved into 30
approved standards.
Standards development a dynamic process
ASTM, founded in 1898, initially had one
committee (E-1, formed in 1904) concerned with
all test methods, and one standard (El, Standard
Methods of Testing), covering all tests. In 1916,
the fifth, and last, part of the El standard
covered macroscopic and microscopic metallo-
graphic procedures in just over two pages.
However, it was soon recognized that one
committee and one test standard could not deal
* Fellow of ASM International
30
w ith the wide range of rapidly evolving test
methods.
Metallography was rather primitive at the
turn of the century; even ·some of the most
elementary aspects were poorly defined. In
1916, ASTM established a new IS-member
committee (Committee E-4 on Magnification
Scales for Micrographs) because it perceived the
problem of developing standard magnification s
as sufficiently unique and important to warrant
specific attention. The name was changed in
1921 to Committee E-4 on Metallograph y,
which expanded the committee's scope to
address other equally, or more importan t
problems, than only establishing standar d
magnifications.
The committee's first standard, developed in
1917, was E2-17T, Tentative Definitions and
Rules Governing the Preparation of Micro-
graphs of Metals and Alloys. (New standards
-until recently - were introduced as "ten-
tative"; thus, the letter T was placed after the
year of introduction.) The three-page-plus standard
consisted of three sections: standard magni-
fications, lenses, and grain size. The section on
grain size did not detail the measuremen t
methods, but only suggested certain application
methods for equiaxed or elongated grains.
Revisions to E2 followed as needs were
identified. Details on the Jeffries planimetric
measurement method were added in 1920, and
in 1924, sections on photographic practices and
radiography were added, increasing the stan-
dard to eight pages. In 1927, the section on
radiography was deleted and a section titled
Recommended Practice for the Care of the Eyes
When Using a Metallographic Microscope
(written by William L. Patterson of Bausch &
Lomb Optical Co.) was added- the committee's
first effort at addressing the safety aspects of
metallography. A grain-size chart (the first
standard chart) was added in 1930, consisting of
ten photomicrographs of brass, i.e., a twinned
austenitic structure at 75X magnification
prepared by a grain-contrast etch. The chart was
developed by a special committee comprising
C.H. Davis (American Brass Co.), H.S. Rawdon
(U.S. Bureau of Standards), Edgar H. Dix, Jr.
(Aluminum Co. of America), and Francis F.
ADVANCED MATERIALS & PROCESSES 11190
 E-4 Standards by Subcommittee Jurisdiction
E.04.01 on Sample Selection and Preparation
and Photography
• E 3-80 1 Standard Methods of Preparation of Metal-
lographic Specimens
• E 340-87 Standard Test Method for Macroetching
Metals and Alloys
• E 381-79 Standard Method of Macroetch Testing,
Inspection; and Rating Steel Products, Comprising
Bars, Billets, Blooms and Forgings
• E 407-70 Standard Test Methods for Microetching
Metals and Alloys
• E 768-80 Standard Practice for Preparing and Evalu-
ating Specimens for Automatic Inclusion Assessment
of Steel
• E 883-86 Standard Guide for Metallographic Photo-
micrography
• E 1180-87 Standard Practice for Preparing Sulfur Prints
o for Macrostructural Examination
• E 1351-90 Standard Practice for Production and Evalu-
ation of Field Metallographic Replicas
E.04.02 on Metallographic Terminology and Nomenclature
of Phase Diagrams
• E 7-89 Standard Terminology Relating to Metal-
lography
• E 157-88 Standard Practice for Assigning Crystal-
lographic Phase Designations in Metallic Systems
• E 391-83 Standard Practice for Presentation of Phase
Diagrams
E.04.05 on Microindentation Hardness Testing
• E 384-84 Standard Test Method for Microhardness of
Materials
E.04.08 on Grain Size
• E 112-88 Standard Test Methods for Determining
Average Grain Size
• E 930-83 Standard Test Methods for Estimating the
Largest Grain Observed in a Metallographic Section
(ALA Grain Size)
• E 1181-87 Standard Test Methods for Characterizing
Duplex Grain Sizes
E.04.09 on Inclusions
• E 45-87 Standard Practice for Determining the Inclusion
Content of Steel
E.04.11 on X-Ray and Electron Metallography
• E 81-89 Standard Test Method for Preparing Quan-
titative Pole Figures of Metals
• E 82-63 Standard Method for Determining the Orien-
tation of a Metal Crystal
• E 766-86 Standard Practice for Calibrating the Magni-
fication of SEM Using NBS-SRM-484
• E 963-83 Standard Practice for Electrolytic Extraction of
Phases from Ni and Ni-Fe Base Superalloys Using a
Hydrochloric-Methanol Electrolyte
• E975-84 Standard Practice for X-Ray Determination of
Retained Austenite in Steel with Near Random
Crystallographic Orientation
• E 986-86 Standard Practice for Scanning Electron
Microscope Performance Characterization
ADVANCED MATERIALS & PROCESSES 11 /90
E.04.14 on Quantitative Metallography
• E 562-89 Standard Practice for Determining Volume
Fraction by Systematic Manual Point Count
• E 1077-85 Standard Test Methods for Estimating the
Depth of Decarburization of Steel Specimens
• E 1122-86 Standard Practice for Obtaining JK Inclusion
Ratings Using Automatic Image Analysis
• E 1182-87 Standard Test Method for Measurement of
Surface Layer Thickness by Radial Sectioning
• E 1245-89 Standard Practice for Determining Inclusion
Content of Steel and Other Metals by Automatic
Image Analysis
• E 1268-88 Standard Practice for Assessing the Degree
of Banding or Orientation of Microstructures
• E 1382-90 Standard Test Methods for Determining the
Average Grain Size Using Semiautomatic and Auto-
matic Image Analysis (in process)
E.04.17 on Laboratory Evaluation and Safety
• E 807-81 Standard Practice for Metallographic Labo-
ratory Evaluation
1
The las/two digits give either the year of adoption or the year of the latest
revision, but not the last year of reapproval if no changes were made.
ASTM E-4 Officers
Chairman- George F. VanderVoort
(Carpenter Technology Corp.)
1st Vice Chairman - Donald R. Green
(Cytemp Specialty Steel)
2nd Vice Chairman - Robert S. Graham
(Ford Motor Co.)
Secretary - Richard K. Wilson
(Inco Alloys International)
Membership Secretary - Thomas N. Rouns
(Aluminum Co. of America)
Technical Subcommittee Chairpersons
E04.01 on Sample Selection and Preparation and Photo-
graphy - Samuel M. Purdy (National Steel Corp.)
E04.02 on Metallographic Terminology and Nomenclature
of Phase Diagrams - Robert S. Graham
(ford Motor Co.J
E04.05 on Microindentation Hardness- Francis J, Toye Jr.
(l..eco Corp.)
E04.08 on Grain Size- Francis J. Warmuth (Cameron Forge Co.)
E04.09 on Inclusions -Albert V. Brandemarte
(David Taylor Research Center)
E04.11 on X-Ray and Electron Metallography - Albert
Szirmae (U.S. Steel Corp.)
E04.14 on Quantitive Metallography - George F. Vander
Voort (Carpenter Technology Corp.)
E04.17 on Laboratory Evaluation and Safety - Linda K.
Kern (Kaiser Aluminum)
31
,.____,. . . Grain structures, etched appearance complicate
grain-size measurement
Ferrite grains in a nonheat-treated or
nonhardenable body-centered cubic (bee)
metal or alloy do not contain annealing
twins, but can contain deformation twins,
as well as second-phase constituents
(carbides in this low-carbon sheet steel, for
example). Etching with nita/ did not reveal
all of the grain boundaries; those that are
visible vary in darkness and width. These
factors are a minor nuisance for manual
grain-size rating and a significant prob-
lem for automqpc rating.
Whereas electrolytically etched 316L
(Figure d) reveals nearly all the grain
boundaries but no twins, tint etching
(20 % aqueous HCI plus 2% NH4FHF
and 0.8 % Na2S20sJofthesamespecimen
reveals the twins and grains by color
contrast.
32
In this microstructure of a single-phase
austenitic alloy (L605) containing an-
nealing twins, grain boundaries are
revealed as dark lines, by a so-called "flat
etch," similar to that in Figure a. Such
alloys are very difficult to etch so that all
grain boundaries are visible, a common
problem that makes it very difficult to
measure grain size with high precision.
Also, twin boundaries must be ignored
when rating grain size, which is difficult,
especially when using image analysis. (Not
all austenitic alloys have annealing twins;
aluminum alloys rarely are twinned.)
The McQuaid-Ehn test is used to
determine if a carbon or alloy steel is
inherently fine grained. After a specimen
is given a standard carburizing treatment,
a nita/ etch reveals a cementite network
around the austenite grains present at the
end of the carburizing cycle, and a rating is
assigned based on the E112 chart having
the same contrast. However, this is not a
good structure from which to make actual
measurements, especially if using image
analysis.
ADVANCED MATERIALS & PROCESSES 11/90
Austenitic alloys can be etched with
reagents that produce grain contrast or
color variations as a function of their
crystallographic orientation, such as in
this twinned austenitic structure of cart-
ridge brass that was etched producing
grains with different contrast in black and
white. All grains are revealed, unlike the
flat-etched specimen in Figure b. While
this structure is easy to rate by the
comparison method if the grain-size chart
depicts grains etched in the same manner,
it is virtually impossible to measure the
grain size of this structure by automatic
image analysis.
It is necessary to have the cementite
network around austenite grain boundaries
sufficiently dark to use image analysis to
measure grain size in a McQuaid-Ehn
test. Beraha's sodium-molybdate tint etch
was used to darken the cementite in this
structure, but the familiar alkaline sodium
picrate etch also works well.

,,
{
To measure twinned austenitic grain
structure by image analysis, it is necessary
to either suppress the etching of twins or be
able to identify and ignore them. Also, all
grain boundaries must be revealed and
identifiable. The best solution is to use an
etchant that reveals only the grain
boundaries, such as with this AISI 316L
stainless steel, electrolytically etched with
60% nitric acid in water (Pt cathode, 0.8
V de, 45 sec)
ADVANCED MATERIALS & PROCESSES ll /90
The dynamic process in action
All committee members are volunteers, either a producer,
user, or general-interest member, and standards are de-
veloped by the consensus approach. Each committee com-
prises subcommittees devoted to specific materials, topics, or
tasks. A specification or standard test method is developed by
a small group of persons in a task group under the relevant
subcommittee. When the task group reaches a consensus, the
document is submitted to the subcommittee for a vote. If
approved, it is submitted to the full committee for a vote, and
upon their approval, it is submitted to the entire ASTM
membership for voting. Members can critique the document
via comments or negative votes at any phase of the process,
most commonly at the subcommittee level; all items must be
resolved before reballotting the document.
A document is assigned a designation number when it
passes the three ballots. Test methods usually begin with the
letter "E" followed by a sequential number (now around
1400). The designation number is followed by a dash and the
last two numbers of the year in which it was approved.
Each specification must be reexamined every five years and
either be reapproved as is, be revised, or be withdrawn if
obsolete. These events occur through the same ballot process.
(Users of such standards should recognize this and keep
abreast of the revisions.)
Along with keeping existing standards technically up-to-
date, a task group revises the structure of a document as
ASTM guidelines change. As an example, ASTM requested
committees to develop information concerning the precision
and bias inherent in standard test methods, chiefly those that
produce numerical data. To generate this information, an
interlaboratory round-robin test program usually is con-
ducted. The test method is applied to evaluate several
specimens whose attributes cover most of the test range and a
large number of people in different companies and labora-
tories perform measurements according to the standard. In
some instances, the true values for the test specimens used in
the round robin are known, but usually they are not; this is a
common problem.
For example, if a round robin is conducted to determine the
precision and bias associated with grain-size measurement,
there is no access to specimens having a known certified grain
size from an organization like the National Institute of
Standards and Technology, NIST (formerly NBS). Instead,
the task group selects from their own sources several
specimens covering a wide range of grain sizes. To simplify
the process, photomicrographs can be used so that variations
within the specimen or preparation differences are not a
factor. Then, many persons rate the grain size of the
specimens or photomicrographs, and the results are examined
for overall agreement, for the spread of results around the
mean (precision}, or for consistent variations by certain raters
(bias). The objective is that the study will reveal those
experimental factors that degrade the precision or cause bias.
Based on the intention of computerizing all standards in the
future, another very recent change in ASTM standards is the
incorporation of a key-word section into each standard; an
essential component of any computerized system. The section
contains a listing of up to about a dozen words or phrases that
might be used in an index to identify a particular standard.
33
 Assorted grain sizes cause assorted problems
Grain-size measurement is relatively straightforward (with a properly
etched specimen) when the microstructure contains equiaxed grains
having a uniform size distribution, i.e., if a single peak is observed that is
symmetrical in shape when a frequency histogram of the grain diameters,
intercept lengths, or areas is plotted using a logarithmic dimension scale.
However, there are occasions where more complex distributions are
observed, often in specimens where recrystallization is incomplete, or at
the onset of rapid grain growth. E112 (Standard Test Methods for
Determining Average Grain Size) is not well suited for such specimens, and
either E930 (Standard Test Methods for Estimating the Largest Grain
Observed in a Metallographic Section, ALA Grain Size) or E1181 (Standard
ASTM Test Methods for Characterizing Duplex Grain Sizes) must be used -
usually the latter.
subcommittees The grain size of such specimens should not be described by an average
create standards value because there possibly will be no grains the size of the average value
in the specimen, or the chosen average value may be within one of the
and are responsible "tails" of the two grain-size distributions. The best approach is to
for their determine the area percentage of each grain-size distribution and the
average grain size of each distribution in specimens having a duplex or
periodic review. bimodal grain size distribution, as described in E1181.

The microstructure of an experimental
hot-work tool steel that was austenitized at
1,080° C reveals the prior-austenite grain
boundaries, which, except for one very
large grain, are from a single distribution.
The grain size of the very large "rogue"
grain can be determined using E93 0, and
the rest of the grains using E112.
Microstructure of A286 steel showing
the onset of grain growth. These are
twinned austenite grains revealed by a
grain-contrast etch, rather than a flat etch
as in Figure aa. E9 3 0 can be used to
measure the largest of these grains, and
E112 to measure the fine region, or the
approaches outlined in E1181 can be used
for the entire structure.
The duplex nature of grain-size distri-
bution can be highly segregated or the two
distributions can be intermixed. This
microstructure shows a relatively well
mired bimodal distribution of grain sizes
in this superalloy specimen having a flat
etch. Annealing twins also are visible.

A segregated form of a duplex grain-size
condition, termed "necklace" type, in a
highly alloyed stainless steel that has not
been fully recrystallized. The fine re-
crystallized grains surround the large
unrecrystallized grains in this transverse
view.
Longitudinal view of a necklace-type
duplex condition in a stainless steel
specimen.
The amounts of the fine and coarse
grains in a duplex grain-size condition can
vary considerably. The percentage of the
number of grains of each type is sig-
nificantly different than the area or volume
percentage of each type. The microstr~c­
ture of this nickel-base superalloy contarns
an approximately equal area percentage of
fine and coarse grains.
 Lucas (Bell Telephone Laboratories).
In 1931, a special subcommittee (chaired by
C.J. Tobin, General Motors Corp.), formed to
study grain characteristics of steels, adopted the
McQuaid-Ehn carburizing test to evaluate
grain-growth characteristics of steel using a
comparison chart. The proposed method was
approved as standard E19-33T, Classific'ation of
Austenite Grain Size in Steels. Grain size was
defined in terms of the number of grains per
square inch at 100X. The chart was widely
criticized as inaccurate, and eventually was
dropped.
A revision of E19 with the addition of a
noncarburizing test was the objective of Oscar
E. Harder (Battelle Memorial Institute) when he
became chairman of the subcommittee in 1936; a
goal not realized. Marcus A. Grossman (Car-
negie-Illinois Steel Co.) became chairman the
following year, and in 1938, the group became
Subcommittee VIII on Grain Size. (Grossman,
famous for his work on hardenability, remained
1- Microstructure of a low-carbon sheet-
10 steel specimen illustrating an extremely
is segregated duplex grain-size condition.
11 Grain growth has occurred at two
locations along the surface of the specimen.
se
Example of a banded or layered duplex
:n condition due to the influence of segregation
't e in a ferritic stainless steel plate specimen,
?- longitudinal view. Note the very long, thin
u unrecrystallized grain.
c-
1S
of
chairman until his death in 1952.)
Sub VIII formed three sections (the term "task
group" was not used at that time), referred to as ASTM
A, B, and C. Section A, chaired by Grossman,
was concerned with improving E19 on austenite
develops
grain size of steels. Section B, chaired by R. Earl standards
Penrod (Bethlehem Steel's Johnstown Plant), by the
was to develop a ferrite grain-size rating method
and chart. Section C, chaired by Carl Samans consensus
(American Optical Co., later with Standard Oil approach
Co. of Indiana), had the task of developing
charts for nonferrous metals and alloys that through
could not be rated using the grain-size chart for volunteer
brass in E2 . Both the grain-size chart for brass
and the grain-size measurement information committee
were deleted from E2 in its 1949 revision and members.
incorporated, together with two additional
grain-size photomicrographs, into the new
standard E79-49T, Methods for Estimating The
Average Grain Size of Wrought Copper and
Copper-Base Alloys. E2 was discontinued in
1984 when E883 (Standard Guide for Metal-
lographic Photomicrography) was introduced.
Section B produced E89-50T, Methods for
Estimating the Average Ferrite Grain Size of
Low-Carbon Steels, with a chart of eight
photomicrographs depicting ferrite grain struc-
tures as revealed by nital etching. This was the
first chart to define grain size in terms of the
now familiar ASTM grain-size numbers (1 to 8
in this chart).
Section C produced E91-51T, Methods for
Estimating the Average Grain Size of Non-
Ferrous Metals, Other Than Copper, and Their
Alloys, consisting of two charts: one for twinned
alloys and one for non twinned alloys. Each chart
had 17 photomicrographs representing ASTM
grain sizes from 2 to 10.
While standards E19, E79, E89, and E91
covered different aspects of grain-size meas-
urement, each also shared many common
points, which led to the combination of the four
standards in 1955 into a single standard, E112,
Methods for Estimating the Average Grain Size
of Metals. Since its adoption in 1961, E112 has
been revised nine times and is currently under
scrutiny for further refinement. One of the
most widely cited ASTM standards, E112 is
primarily concerned with grain-size measure-
ment of equiaxed (nondeformed) grains, al-
though it contains some information about
grain-size measurement of grains elongated by
processing.
However, there are situations where E112 is
not helpful and other standards have been
developed. For example, certain alloys have a
bimodal rather than a uniform grain-size
distribution. Two ASTM standard test methods
that deal with such structures are: E930,
Standard Test Methods for Estimating the
Largest Grain Observed in a Metallographic
Section (ALA Grain Size), and E1181, Standard
Test Methods for Characterizing Duplex Grain
Sizes.
Due to the increase in popularity of using
37
 image analysis to determine grain size, a new
standard, E1382, Standard Test Methods for
All Determining the Average Grain Size Using
specifications Semiautomatic and Automatic Image Analysis,
has just completed the balloting process. This
must be standard describes a number of equivalent
reexamined approaches for measuring grains size using both
tablet digitizer systems and fully automatic
every five systems.
years
Work in other areas
While standardizing grain-size-measurement
methods has been one of the most visible
Committee E-4 accomplishments, other stan-
dardization work also has been done. For
example, results of interlaboratory "round
robins" were used to prepare detailed precision
and bias sections for E384 (Standard Test
Method for Microhardness of Materials) and
E562 (Standard Practice for Determining
Volume Fraction by Systematic Manual Point
Count). E384 also is currently undergoing a
major revision, wherein the term "microhard-
ness" is being replaced throughout by "micro-
indentation hardness." The former, although
widely used, might suggest that the hardness is
extremely small rather than the indent.
E381 (Standard Method of Macroetch Test-
ing, Inspection, and Rating Steel Products,
Comprising Bars, Billets, Blooms, and Forgings)
also is being revised. Originally developed to
evaluate hot-worked ingot cast material, the
Circle 24 on reader service card
38
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standard is not suitable for evaluating many
aspects of continuously cast products. New
charts are being developed to aid in classification
and interpretation of such material both in the
as-cast and hot-worked conditions, and a section
is being added to define terms related to both
conditions.
E45 (Standard Practice for Determining the
Inclusion Content of Steel) is being updated so
that it will be more useful in evaluating today's
steels, particularly calcium-treated steels. The
current standard, consisting of four approaches
to assess inclusion content (three use com-
parison charts), is widely referenced by other
specifications. Development of the image-ana-
lysis approach to obtain E45 inclusion ratings
according to E1122 (Standard Practice for
Obtaining JK Inclusion Ratings Using Auto-
matic Image Analysis) shows that some aspects
of the E45 inclusion-rating methods need to be
defined more rigorously. Interlaboratory round
robins also have demonstrated that there is a
problem for some operators in separating type A
from type C inclusions. Also, for the novice
rater, E45 needs to be more informative
regarding the distinctions between the four
basic inclusion types. These, and other, pro-
blems are being addressed by a task group
working on the revision of E45. A stereology-
based approach for measuring the inclusion
content (or the amount of any discrete second
phase) by image analysis is described in E1245.
In addition to revising standards, E-4 has a
number of new projects underway. The growth
in the use of image-analysis equipment, as well
as increasing equipment capabilities over the
past 27 years, has generated a great deal of work
in this area by Sub 14 on Quantitative
Metallography (founded in 1960). Sub 14's first
standard, E562 (Standard Test Method for
Determining Volume Fraction by Systematic
Manual Point Count), was adopted in 1976 and
has been revised twice, most recently in 1989
when a detailed precision and bias section was
added. Sub 14 now has three image-analysis
standards.
Among other projects being worked on is one
in which a test slide is being developed for use in
evaluating image-analysis programs and their
calibration, and one in which a standard for
evaluating the degree of nodularity of graphite
is being written. Sub 11 on X-ray and Electron
Metallography is presently analyzing results of
an interlaboratory round robin on quantitative
energy-dispersive X-ray analysis (EDXA). This
information will be used to develop a standard
on EDXA work. II
How useful did you find the information presented in this article?
Very useful, Circle 326 Of general interest, Circle 327
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ADVANCED MATERIALS & PROCESSES 11 /90