Standards for Metallography

Standards for Metallography

George F. Vander Voort
Director, Research & Technology
Buehler Ltd.
Lake Bluff, Illinois USA
Why Do We Need Standards?
Standards are prepared by experts on the subject and they
represent a summary of the current state of knowledge on the
best practices to use.
If everyone uses the same, best method then results between
laboratories will have better reproducibility (i.e., agreement
between laboratories)
National and international standards are continuously revised
and kept up-to-date with changes in technology
Types of Standards
Types of Standards
Company standards relate best to the local needs, but the
methods may be poorly developed and defined
National standards developed by industry/academic experts
in the particular field but the practices and quality of the
standards vary from country to country
International standards these are written, and balloted in a
number of countries with leading technology and should
represent the best ideas on a given test method (ISO)
ISO standards tend to be short in length and contain only the
basic information required
ASTM test method standards give more background details
and have precision and bias data based on interlaboratory test
programs (round robins)
ISO Metallography Standards
ISO Metallography Standards
21 standards on hardness testing (8 on HV, 8 on HK and 6 on
HRC) too many! HV test is broken into standards for loads <
200gf and loads >200 gf
3 Grain Size Methods (one on Fe, one on Cu)
2 on Graphite Characterization (flake vs nodular)
7 on Coating Thickness Measurement
1 on the Microstructure of Hard Metals
1 on the Sulfur Print Test
1 on Carbide Segregation in Bearing Steels
1 on Manual Point Counting
2 on Nonmetallic Inclusion Rating (macro vs micro)
How are ISO Standards Created?
How are ISO Standards Created?
Committees set up with representatives from member and
observer countries (later rarely come to meetings)
Each committee chaired by a country, the secretariat
usually a national standards writing organization
Representatives are often bureaucrats who bring specific
technical experts to the meeting depending upon the topics
Committees meet irregularly, when there is business
All standards must be reviewed every 5 years
If a standard must be revised, it is done usually by one
person (and anyone they wish to utilize) from one country
Revisions are only balloted within the committee
Creating an ASTM Standard
Creating an ASTM Standard
Each of the more than 130 ASTM committees can create
standards (of various types) on their subject of interest.
Committee E-4 on Metallography writes test methods
standards, so the committee need not be balanced between
people representing producers and purchasers.
A standard is created when a need is shown to exist and a
task group can be formed with enough people with the
needed expertise to write a draft
The draft is balloted in the task group until all agree that it
is acceptable to go to Subcommittee ballot
After it passes subcommittee ballot, it must pass a
committee ballot, and then a society ballot.
ASTM Standards
ASTM Standards

Upkeep Process
Upkeep Process
Every ASTM standard must be reviewed every 5 years
A task group is assigned to review the standard
It decides if the standard is acceptable as written, if
technology has changed and it must be modified, or that the
standard is of no value and can be made obsolete
For any of the above actions, a ballot is required. If it is to
be revised, a task group is given the job to make the
necessary changes. The revised draft must go through ballots
within the task group, the subcommittee, the committee and
the society
If it is to be withdrawn or re-approved as is, this decision
must be balloted, but it is a simple ballot usually
ASTM Metallography Standards
ASTM Metallography Standards
Terminology (E7)
Specimen Preparation (E3, E340, E407, E768,
E1558, E1920, E2015)
Macrostructural Evaluation (E381, E1180)
Light Microscopy (E883, E1951)
Quantitative Metallography (E45, E112, E562,
E930, E1077, E1122, E1181, E1245, E1268, E1382,
E2109)
XRD, SEM, TEM (E81, E82, E766, E963, E975,
E986, E2142)
Microindentation Hardness Testing (E384)
E
E
-
-
4 Standards for Quantitative Metallography
4 Standards for Quantitative Metallography
Inclusion rating
Grain Size
Volume Fraction
Characterization of Second Phases
Case Depth/Decarburization
Degree of Banding
E
E
-
-
4 Standards for Quantitative Metallography
4 Standards for Quantitative Metallography
Determine for the method defined its
Precision and Bias
(accuracy usually cannot be determined)
Using Interlaboratory Test Programs,
Commonly called round robins
Quantitative Metallography
Numerical measurements of microstructural features
1. Surface Gradients
Standard metrology methods
2. Matrix Microstructures
Stereological Measurements
Metrology Measurements
STEREOLOGY
Extrapolation of measurements made on
a two-dimensional sectioning plane to
determine the three-dimensional
characteristics of the microstructure
Measurements may be 0-, 1-, or 2-
dimensional (i.e., points, lines, areas)
STEREOLOGY
Matrix Microstructural Measurements
Planar (flat) Surface Images
Non-planar (curved) Surface Images
Projected Images
Planar Surface Images
Flat, polished and etched surfaces
require no additional corrections and
are the simplest to employ. Surface
relief in preparation must be
minimized and etching depth must be
minimal.
Non-Planar Surface Images
SEM images of fractures depict the rough
surface as being flat. However, the surfaces
are not flat but exhibit hills and valleys that
vary with the fracture mode and
mechanism. The measurements must be
corrected by determining the surface
roughness by, for example, using vertical
sections. Otherwise, all measurements are
biased.
Projected Images
Images created using transmitted light or
electrons (as in TEM thin foils) sense the
structure within a volume of material.
Hence, measurements reflect data in
volume and the results must be corrected
knowing the thickness or depth of the
image plane. If not, biased data will be
obtained.
Statistical Analysis
Mean (average)
Standard Deviation
95% Confidence Interval
% Relative Accuracy
Tests to evaluate the significance of
differences between mean values
Statistical Analysis
Statistical precision of the data is
mainly a function of the number of
measurements made. This is why
image analysis can produce
significantly better data than
manual procedures.
Statistical Analysis
Mean (Average)
X =
X
i
N
X
i
are the individual values and
N is the number of measurements
Statistical Analysis
Standard Deviation distribution of the
individual values around the mean
S = [ ]
( x
i
x)
2
N - 1
1/2
Statistical Analysis
95% Confidence Interval
95% CI =
ts
(N)
1/2
t is the Students t value for a 95% CI and for
N-1 degrees of freedom
Statistical Analysis
% Relative Accuracy
%RA = x 100
95% CI
X
10% RA is a good target, especially for manual
measurements, but is difficult to achieve when
the volume fraction is <2%, even with image
analysis equipment.
Accuracy vs. Precision
To determine the accuracy of a
measurement, we must know the true value
by some reference method. For
microstructural measurements, we never
know the true value by any independent
referee method. Therefore, we can only
assess the precision of our measurements in
terms of the scatter around the mean value.
Specimen Preparation
Image analyzers require correctly
prepared specimens - better quality
than for manual measurements.
You cannot measure what cannot be seen!
Stereological Symbols
P = Point
L = Line
A = Area (planar)
S = Surface (curved)
V = Volume
N = Number
Symbols can be combined, e.g., V
V
, N
A
, L
A
, S
V
The following slide shows a
synthetic microstructure
consisting of 30 spherical
particles with three different
diameters to illustrate
certain measurements
Volume Fraction A Measure of
the Concentration of a Second
Phase Constituent
V
V
=
V

V
T
But, there is no simple way to directly measure
the volume per unit volume of a constituent!
Volume fraction can be assessed
from the area fraction, linear
fraction or point fraction, that is -
V
V
= A
A
= L
L
= P
P
For manual measurements, P
P
is the easiest
method and most efficient (i.e., best
precision for a given amount of work)
Areal Analysis Area Fraction
Earliest measurement procedure, used
with minerals. Can only be done
manually on structures that are coarse
and consist of simple geometric shapes.
The method is very precise for a given
field, but too time consuming to measure
a large number of fields.
A
A
=
A
A

A
T
1
1 1
2
3 3
2
2 4
4
5 5
6
7
6
3
8
4
7
8
9
5
10
9
6
14
11
10
12 13
Calculate the Area Fraction, A
A
Calculate the area of each spherical particle
(circular in cross section) based on a diameter
measurement and a count of the number of
each size particle. We will assume that the
image is at 500X magnification. The
diameters of the three circular particles
are:12.6, 21.6 and 34 m. The areas of the
circular particles are: 124.69, 366.44 and
907.92 m
2
. The test area measures 512 by
380 m or 194560 m
2
.
Calculate the Area Fraction, A
A
A
A
=
[(6x907.92) + (10x366.44) + (14x124.69)]
(512 x 380)
A
A
= 0.056 = 5.6%
Point Fraction Point Counting
ASTM E 562
Superimpose a grid composed of points over
the microstructure. In practice, points are hard
to see, so we use crosses or intersecting vertical
and horizontal test lines. The intersection is the
point. The point must be in the constituent to
be a hit. If it is a tangent hit, count it as
one-half. Calculate P
P
by:
P
P
=
P

P
T
Point Counting Grids
The optimum number of points in a point
counting grid is a function of the volume
fraction to be measured and is determined from
the equation, P = 3/V
V
, where the volume
fraction is a fraction, not a percentage. So, as
V
V
decreases from 0.5 (50%) to 0.01 (1%), P
varies from 6 to 300.
The following 100-point grid is convenient to
use as each hit is 1%.
Use of the Point-Counting Grid
The grid consists of ten horizontal and
vertical lines, yielding 100 points (the
intersection points of the lines). This is
superimposed over the microstructure and
the image is scanned, usually from upper
left to the lower right, while noting the
number of points that are inside the
constituent of interest, and those on phase
boundaries (weighed as one-half a hit).
This is repeated for N fields. Then, the point
fraction is calculated and is an estimate of
the volume fraction.
1
2
3
5
4
7
Calculation of P
P
In this example there were 7hits where
the points were inside the constituent of
interest, and no tangent hits. So, the point
fraction is calculated as:
P
P
= = 0.07 = 7%
7
100
To obtain good data, more fields must be evaluated.
Image Analysis vs. Manual
For manual work, to obtain the best
precision, point count more fields as the
field-to-field variability has a greater
influence on precision than the precision in
measuring a single field. The adage is do
more, less well that is, put less effort into
measuring each field and do more fields.
For IA work, all of the pixels in the field are
used. Thus, the precision per field is higher,
but the time per field is very small. Hence,
even if N is the same, the %RA is better.
Intersections Per Unit Length, P
L
P
L
is a measure of the number of point
intersections with phase or grain
boundaries per unit length of test line. It
is calculated from:
P
L
=
P

L
T
P

is the number of intersections and L

T
is the true
line length (line length/magnification)
Intersections/Unit Length, P
L
To illustrate this calculation, let us
superimpose a series of horizontal test
lines, such as used in the lineal analysis,
over the synthetic microstructure.
Intersections/Unit Length, P
L
The point intersections are indicated in
the next slide.
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
20
22
23
24
25
26
27
28
29
30
31
32
33
34
35
19
21
Intersections/Unit Length, P
L
In the example, P

is 35. If each of
the 10 lines is 256 mm long, and
the magnification is 500X, then,
L
T
is 5.12 mm, and
P
L
= = 6.84 mm
-1
35
5.12
Interceptions Per Unit Length, N
L
N
L
is a measure of the number of
interceptions with phase or grain
particles per unit length of test line. It is
calculated from:
N
L
=
N

L
T
N

is the number of interceptions and L

T
is the
true line length (line length/magnification)
Interceptions/Unit Length, N
L
To illustrate this calculation, let us
superimpose a series of horizontal test
lines, such as used in the lineal analysis,
over the synthetic microstructure.
Interceptions/Unit Length, N
L
The particle interceptions are indicated
in the next slide.
1
2 3
4
5
6
7.5
7
8.5
9.5
10
10.5 11.5
12.5
13.5
14.5
15.5
17.5
16.5
Interceptions/Unit Length, N
L
In the example, N

is 17.5. If each
of the 10 lines is 256 mm long,
and the magnification is 500X,
then, L
T
is 5.12 mm, and
N
L
= = 3.42 mm
-1
17.5
5.12
Number Per Unit Area, N
A
The number of particles per unit area,
N
A
, is a measure of the quantity of
particles, that is the number density.
N
A
is related to the number per unit
volume, N
V
, which can only be
determined by serial sectioning. It is
determined by:
N
A
=
N

A
T
Number Per Unit Area, N
A
To illustrate the determination of N
A
, let
us count the number of particles in our
synthetic microstructure and then divide
by the test area. The synthetic
microstructure with 30 particles is shown
in the next slide.
Number Per Unit Area, N
A
The test area measures 256 x 190 mm and
the magnification is 500X. Therefore, N
A
is given by 30 particles divided by the
true test area:
N
A
= = 154.2 mm
-2
(256/500)x(190/500)
30
Average Particle Area, A
The average particle size, as measured by
the area, can be determined from a ration
of the field measurements, A
A
and N
A
,
without use of individual particle area
measurements from:
A =
A
A
N
A
Average Particle Area, A
The area fraction was determined
previously by areal analysis, lineal
analysis and point counting, that is, A
A
,
L
L
and P
P
. Of these, the A
A
value is the
most precise. N
A
was also determined. So,
the average cross-sectional area of the
particles is:
A = = 0.0003632 = 363.2 m
2
0.056
154.2
Average Particle Area, A
Using image analysis, we can measure the
area of each particle, add all the areas, and
divide by the number of particles. As we
have particles with a perfect circular cross-
section, we can measure the diameter and
calculate the area of each particle. Then,
sum the areas and divide by the number of
particles. The average area is:
A =
A
i
N

Average Particle Area, A

A = = 361.9 m
2
10857.6
30
Comparison of Average Areas
Average area based on the area fraction divided
by the number per unit area = 363.2 m
2
Average area based on actual measurements
was 361.9 m
2
363.2 361.9
Mean Center-to-Center Spacing,
The mean spacing between particle
centers, in all directions, is given simply
by the reciprocal of N
L
:
=
1
N
L
Mean Center-to-Center Spacing,
In the case of our synthetic
microstructure, N
L
was determined as
3.42 interceptions per mm. So, is:
= = 0.2924 mm = 292.4 m
1
3.42
Mean Edge-to-Edge Spacing,
The mean edge-to-edge spacing between
particles, known as the mean free path, is a
good structure-sensitive parameter. is
calculated from:
=
1 - A
A
N
L
Mean Edge-to-Edge Spacing,
In the case of our synthetic microstructure,
A
A
and N
L
were determined. So, is:
= = 0.276 mm = 276m
1 0.056
3.42
The MFP is a very structure-sensitive parameter used in
ASTM E 1245 to characterize second-phase particles
Degree of Orientation,
=
(P
L
) - (P
L
)||
(P
L
) + 0.571(P
L
)||
Usually expressed as a percentage (%)
Used in ASTM E 1268 to assess the degree of banding or
orientation in structures viewed on a longitudinal plane
Interlamellar Spacing

r
=
1
N
L

t
=

r
2
Where
r
is the mean random spacing
and
t
is the mean true spacing.
Measure N
L
with random test lines, such as with a circle,
rather than directed test line (perpendicular to lamellae)
Grain Size Measurement
Types of Grain Sizes
Non-twinned(ferrite, BCC metals, Al)
Twinned FCC Metals (austenite, Cu, Ni)
Prior-Austenite
(Parent Phase in Q&T Steels)
Grain Size Measurements
Number of Grains/inch
2
at 100X: G
Number of Grains/mm
2
at 1X: N
A
Average Grain Area, m
2
: A
Average Grain Diameter, m: d
Mean Lineal Intercept Length, m: l
Grain Size Measurement Methods
Comparison Chart Ratings
Shepherd Fracture Grain Size Ratings
Jeffries Planimetric Grain Size
Heyn/Hilliard/Abrams Intercept Grain Size
Snyder-Graff Intercept Grain Size
2D to 3D Grain Size distribution Methods
Definition of ASTM Grain Size
n = 2
G-1
n = number of grains/in
2
at 100X
G = ASTM Grain Size Number
ASTM Grain Size, G
G n G n
1 1 6 32
2 2 7 64
3 4 8 128
4 8 9 256
5 16 10 512
ASTM Standards for Grain Size
ASTM E 112: For equiaxed, single-
phase grain structures
ASTM E 930: For grain structures
with an occasional very large grain
ASTM E 1181: For characterizing
duplex grain structures
ASTM E 1382: For image analysis
measurements of grain size, any type
Comparison Chart Ratings
Look at a properly etched microstructure,
using the same magnification as the chart, and
pick out the chart picture closest in size to the
test specimen. If the grain structure is very
fine, raise the magnification, pick out the
closest chart picture and correct for the
difference in magnification according to:
G = Chart G + Q
Q = 6.64Log
10
(M/M
b
)
where M is the magnification used and
M
b
is the chart magnification
Jeffries Planimetric Method
n
1
= number of grains completely inside the
test circle
n
2
= number of grains intercepting the
circle
N
A
= f[ n
1
+ (n
2
/2)]
f = Jeffries multiplier
f = magnification
2
/circle area
Jeffries Planimetric Method
Average Grain Area = A =
G = (-3.322LogA) 2.955
1
N
A
n
1
= 68 and n
2
= 41
Jeffries Planimetric Method - Example
For the preceding micrograph,
n
1
= 68 and n
2
= 41
And
f = = = 0.497
M
2
A
100
2
20106.2
Jeffries Planimetric Method - Example
N
A
= f[n
1
+ (n
2
/2)]
N
A
= (0.497)[68 + (41/2)]
N
A
= 44.02 mm
-2
Jeffries Planimetric Method - Example
A = = 0.0227 mm
2
1
N
A
d = (A)
1/2
G = 2.5
Jeffries Planimetric Method - Example
This is an austenitic Mn steel, solution annealed and aged to
precipitate a pearlitic phase on the grain boundaries (at 100X).
There are 43 grains within the circle (n
1
) and there are 25 grains
intersecting the circle (n
2
). The test circles area is 0.5 mm
2
at 1X.
Jeffries Planimetric Method - Example
N
A
= f[n
1
+ (n
2
/2)]
f = [(100
2
)/5000]
N
A
= 2[43 + (25/2)] = 111 mm
-2
G = [3.22Log
10
(111)] 2.954 = 3.8
(Of course, more than one field should be measured to get
good statistical results)
Heyn/Hilliard/Abrams Intercept Method
N = number of grains intercepted
P = number of grain boundary intersections
N
L
=
N
L
T
P
L
=
P
L
T
where L
T
is the true test line length
Heyn/Hilliard/Abrams Intercept Method
Apply a test line over the microstructure
and count the number of grains intercepted
or the number of grain boundary
intersections (easier for a single-phase grain
structure). After you count N or P, divide
that number by the true line length to get
N
L
or P
L
.
Intercept Counts (N)
1/2
1 1
1
1
1
1/2
The test line intercepted 5 whole grains and the line ends fell
in two grains. These are weighted as an interception. So the
total is 6 intercepts (N=6).
Intersection Counts (P)
1 1 1 1 1 1
The test line has intersected 6 grain boundaries. The ends
within the grains are not important in intercept counting.
So, P=6 for the intercept count.
Heyn/Hilliard/Abrams Intercept Method
Mean Lineal Intercept, l = =
1
N
L
1 1
P
L
G = [6.644Log
10
(N
L
or P
L
)] 3.288
G = [-6.644Log
10
(l)] 3.288
Note: Units are in mm
-1
(for N
L
and P
L
) or mm (for l)
Heyn/Hilliard/Abrams Intercept Method
If the grain structure is not equiaxed, but
shows some distortion of the grain shape, use
straight test lines at various angles, or simply
horizontal and vertical with respect to the
deformation axis of the specimen.
Alternatively, you can use test circles, such as
the ASTM three-circle grid (three concentric
circles with a line length of 500 mm). This
test pattern averages the anisotropy.
Heyn/Hilliard/Abrams Intercept Method
Example of three concentric test circles
for point counting.
To illustrate intercept counting, note that there are 41, 25 and 20 grains
intercepted (N) by the three concentric circles.
Intercept Counting Example
L
T
= 11.4 mm
N = 41 + 25 + 20 = 86
N
L
= = 7.54 mm
-1
86
11.4
l = = 0.133 mm
1
7.54
G = [-6.644Log
10
(0.133)] 3.288 = 2.5
Intercept Grain Size Example Single Phase
This is a 100X micrograph of 304 stainless steel etched electrolytically with
60% HNO
3
(0.6 V dc, 120 s, Pt cathode) to suppress etching of the twin
boundaries. The three circles have a total circumference of 500 mm. A count
of the grain boundary intersections yielded 75 (P=75).
Intercept Grain Size Example Single Phase
P
L
= = 15 mm
-1
75
500/100
l = = 0.067 mm
1
15
G = [-6.644Log
10
(0.067)] 3.288 = 4.5
Intercept Method for Two-Constituents
N

= Number of grains intercepted

L
T
= Test line length/Magnification
V
V
= Volume fraction of the phase
l

=
V
V
(L
T
)
N

Intercept Method for Two-Constituents

This 500X micrograph of Ti-6242 was alpha/beta forged and alpha/beta annealed,
then etched with Krolls reagent. The circumference of the three circles is 500 mm.
Point counting revealed an alpha phase volume fraction of 0.485 (48.5%). 76 alpha
grains were intercepted by the three circles.
Intercept Method for Two-Constituents
l

= = 0.006382 mm
(0.485)(500/500)
76
G = [-6.644Log
10
(0.006382)] 3.288 = 11.3
Particle Size Measurement
Six ways to measure particles on a polished cross section.
Particle Size Measurement
Volumetric Diameter, d
V
Diameter of a sphere with the same
volume as the particle
V = d
V
3

6
Particle Size Measurement
Ferets Diameter, d
F
Mean distance between pairs of
parallel tangents to the projected
outline of the particle
Particle Size Measurement
Projected Area Diameter, d
A
Diameter of a circle with the same
area as the projected area of the
particle.
A = d
A
2

4
Particle Size Measurement
Perimeter Diameter, d
P
Diameter of a circle with perimeter
length the same as the projected outline
of the particle
P = d
P
Shape Descriptors
SPHERICAL
Global shaped
(Circular on a cross section
through the particle)
Shape Descriptors
ACICULAR
Needle-like in three dimensions
Shape Descriptors
FLAKY
Irregular plate-like shape
Shape Descriptors
DENDRITIC
Branched,
Tree-like in three dimensions
Shape Descriptors
LENTICULAR
Lens-like shape
Shape Descriptors
FIBROUS
Regular or irregular
Tread-like shape
Shape Descriptors
ANGULAR
Sharp edged or
Roughly polyhedral shaped
Shape Descriptors
GRANULAR
Approximately equidimensional
Irregularly shaped
Shape Descriptors
IRREGULAR
Lacking any symmetry
Shape Factors
Elongation Ratio or
Anisotropy Ratio
AR =
Length
Width
Shape Factors
Sphericity (Roundness)
S =
4A
P
2
S = 1 for a circular feature; S < 1 for other shapes
Sometimes this equation is
reversed
Perimeter Sensitive to
Magnification
Try to use shape factors that do not
require a perimeter measurement,
especially when the particles are
small (<30 pixels/particle)
Perimeter-Free Shape Factor
Measure the maximum Ferets diameter,
d
Fmax
, and calculate the area of the circle
with that diameter.
A
F
= ()
d
Fmax
2
2
SF
PF
=
A
F
A
measured
Degree of Nodularity of Graphite
% Nod. =
100(A
i
with SF 0.6)
A
i
A
i
is the area of a graphite particle
Variations in Graphite Shape
Nodular Iron
Compacted
Graphite Cast Iron
Flake Gray Cast Iron
Magnification bars are
all 100 m long
Shape Factors - Example
Histogram of sphericity shape factors for two flake gray iron specimens, a
compacted graphite specimen and a nodular graphite specimen.
ASTM E 1245
A Stereological Procedure to Characterize
Discrete Second-Phase Particles
Uses field and feature-specific measurements.
While the measurements employ stereological
parameters, they may be made on only one plane,
for example, the longitudinal. If the three-
dimensional values are desired, then additional test
planes must be assessed.
ASTM E 1245
Measure or calculate:
Area Fraction, usually in %
Number per mm
2
, N
A
Average Length in m
Average Area in m
2
Mean Free Path in m
ASTM E 1245
Area fractions of inclusions on three parallel planes, same
specimens, of Alloy 718.
ASTM E 1245
Number per sq. mm of inclusions on three parallel planes, same
specimens, for Alloy 718.
ASTM E 1245
Average area of inclusions on three parallel planes, same
specimens, for Alloy 718
ASTM E 1245
Mean free path of the inclusions on three parallel planes, same
specimens, for Alloy 718.
ASTM E 1245
Sulfide area fractions on 12 specimens taken along an as-cast bar of 303
stainless steel, at the mid-radius location.
ASTM E 1245
Sulfide number per sq. mm taken at 12 locations along an as-cast bar
of 303 stainless steel at the mid-radius location.
ASTM E 1245
Average area of sulfides taken at 12 locations along an as-cast bar of 303
stainless steel, at the mid-radius location.
ASTM E 1245
Mean free path for sulfides at 12 locations along an as-cast bar of 303
stainless steel, at the mid-radius location.
ASTM E 1245
Distribution of area fractions of the sulfides for 106 bars of wrought 303
stainless steel, at the mid-radius location, longitudinal plane.
ASTM E 1245
Distribution of number per sq. mm of sulfides for 106 bars of wrought 303
stainless steel, at the mid-radius location, longitudinal plane.
ASTM E 1245
Distribution of average area of sulfides for 106 bars of wrought 303
stainless steel, at the mid-radius location, longitudinal plane.
ASTM E 1245
Plot of sulfide length vs. area measurements for each of 106 wrought
bar specimens in wrought 303 stainless steel.
Point Counting Inclusions
Point counting of inclusions is tedious and imprecise. This work used 100
fields measured with a 100-point grid, but the 95% confidence limits are
poor, typical for volume fractions below 2%.
Lineal Analysis of Inclusions
A Hurlbut counter was used (one hour per specimen) to measure the lineal
fraction of inclusions. Again, the precision of the measurements is poor.
Image Analysis Inclusion Measurement
Image analysis measurement of the inclusions using 1080 fields (grouped in 12 sets
of 90) gave better precision in less time than the manual measurements.
Image Analysis Inclusion Measurement
Inclusions measured by image analysis using different magnifications (field
sizes) shows the influence of the number of fields on the mean value.
Image Analysis Inclusion Measurement
The relative accuracy of the inclusion volume fractions improved with
increasing number of fields measured and is poorest for the highest
magnification (small field size increases field-to-field variability).
Image Analysis Inclusion Measurement
The relative accuracy of the inclusion area fractions improved (decreased) as
the area measured increased.
Future of Standardization
Future of Standardization
More standards are being created each year due to technology
changes, e.g., due to new materials being developed
More automation is being introduced into test methods and these
changes must be rolled into all standards affected by the
technology changes
Microstructural test methods are moving to quantification by
stereological principles, using image analyzers, rather than using
qualitative chart methods
More statistical analysis procedures are being introduced into
test methods that yield numerical data
Precision and bias information, based on interlaboratory test
programs are being added to standards that produce numerical
data