This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

 
Designation: E562 − 19

Standard Test Method for

Determining Volume Fraction by Systematic Manual Point
Count1
This standard is issued under the fixed designation E562; the number immediately following the designation indicates the year of 

original adopt
original adoption
ion or, in the case of revis
revision,
ion, the year of last revision.
revision. A number in parent
parentheses
heses indicates
indicates the year of last reappr
reapproval.
oval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

INTRODUCTION

Thiss test method

Thi method may be useused
d to det
determ
ermine
ine the vol
volume
ume fraction
fraction of con
constit
stituen
uents
ts in an opa
opaque
que
specimen
specime n usi
using
ng a pol
polish
ished,
ed, pla
planar
nar cro
cross
ss sec
sectio
tion
n by the man
manual
ual poi
point
nt cou
count
nt pro
proced
cedure
ure.. The sam
samee
measurements can be achieved using image analysis per Practice E1245
Practice  E1245..

1. Sco
Scope
pe E407 Practice for Microetching Metals and Alloys
E407 Practice
1.1 Thi
Thiss tes
testt meth
method
od des
descri
cribes
bes a sys
systema
tematic
tic man
manual
ual poi
point
nt E691   Practic
E691 Practicee for Conducting an Interl
Interlabora
aboratory
tory Study to
counti
cou nting
ng pro
proced
cedure
ure for stat
statisti
istical
cally
ly esti
estimat
mating
ing the vol
volume
ume Determine the Precision of a Test Method
fraction of an identifiable constituent or phase from sections E1245   Prac
E1245 Practice
tice for Det
Determ
ermini
ining
ng the Inc
Inclus
lusion
ion or Sec
Second
ond--
through the microstructure by means of a point grid. Phase Constituent
Constituent Conten
Contentt of Metals by Automatic
Automatic Image
Analysis
1.2 The use of automatic
automatic image analysis
analysis to dete
determi
rminene the
volume fraction of constituents is described in Practice E1245
Practice  E1245.. 3. Terminology
1.3
1.3 Th
Thee va
valu
lues
es st
state
ated
d in SI un
unit
itss ar
aree to be re
rega
gard
rded
ed as
3.1   Definitions— For
F or de
definfinititio
ions
ns of te
term
rmss us
used
ed in th
this
is
standard. No other units of measurement are included in this
practice, see Terminology 
Terminology   E7
E7..
standard.
3.2  Definitions of Terms Specific to This Standard:
1.4   This standar
standard d doe
doess not purport
purport to addaddre
ress
ss all of the
safe
safety
ty co
conc
ncer
erns
ns,, if an
anyy, as
asso
soci
ciat
ated
ed wi
with
th its us
use.
e. It is th
thee 3.2.1   point count— the
the total number of points in a test grid
responsibility of the user of this standard to establish appro- that fall within the microstructural
microstructural feature of interest, or on the
 priate safety, health, and environmental practices and deter- feature boundary; for the latter, each test point on the boundary
mine the applicability of regulatory limitations prior to use. is one half a point.
1.5   This inte
interna
rnatio
tional
nal sta
standa
ndard
rd wa
wass dev
develo
eloped
ped in acc
accor
or-- 3.2.2   point
point frac
fraction — th
tion—  thee ra
rati
tio,
o, us
usua
uall
lly
y ex
expr
pres
esse
sedd as a
dance with internationally recognized principles on standard- percentage, of the point count of the phase or constituent of 
izatio
izationn es
esta
tabl
blis
ishe
hedd in th thee De
Deci
cisio
sion
n on Pr Prin
inci
cipl
ples
es fo
forr th
thee interest on the two-dimensional image of an opaque specimen
 Development of International Standard
Standards, s, Guides and Recom- to the numbe
numberr of grid points,
points, which is averag
averaged
ed over  n  fields to
mendations issued by the World Trade Organization Technical produc
pro ducee an unb
unbias
iased
ed esti
estimat
matee of the vol
volume
ume fraction
fraction of the
 Barriers to Trad
Tradee (TBT) Committee. phase or constituent.

2. Refere
Referenced
nced Documents
Documents 3.2.3   stereology— the
the methods developed to obtain informa-
tion about the three-dimensional characteristics of microstruc-
2.1   ASTM Standards:2 tures
tur es bas
baseded upo
upon
n mea
measur
sureme
ements
nts mad
madee on two
two-di
-dimen
mensio
sional
nal
E3 Guide
E3  Guide for Preparation of Metallographic Specimens secti
se ction
onss th
thro
roug
ugh
h a so
solid
lid ma
mater
teria
iall or th
their
eir pr
proj
ojec
ectio
tion
n on a
E7   Terminology Relating to Metallography
E7 surface.
3.2.4   test grid— a transparent sheet or eyepiece reticle with
1
This tes
This testt met
method
hod is und
under
er the jur
jurisd
isdict
iction
ion of AS
ASTM
TM Com
Commit
mittee
tee   E04   on a regular pattern of lines or crosses that is superimposed over
Metallography and is the direct responsibility of Subcommittee E04.14
Subcommittee  E04.14   on Quanti-
the microstructural image for counting microstructural features
tative Metallography.
Current edition approved Aug. 15, 2019. Published September 2019. Originally of intere
interest.
st.
approved
approv ed in 1976. Last previous edition approved in 201 2011
1 as E562 –11–11.. DOI:
10.1520/E0562-19.
3.2.5   volume
volume fraction— th
thee to
fraction—  tota
tall vo
volu
lume
me of a ph
phas
asee or
2
For refere
referenced
nced ASTM stand
standards,
ards, visit the ASTM websi
website,
te, www
www.astm
.astm.org
.org,, or constituent per unit volume of specimen, generally expressed
contact ASTM Customer Service at service@astm.org. For  Annual Book of ASTM  as a percentage.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. 3.3   Symbols:

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  E562 − 19
TABLE 1 95 % Confi
Confidence
dence Interval Multipliers an unbiased statistical estimation of the volume fraction of an
No. of Fields n 
Fields  n    t No. of Fields  n    t phase   (1,   2,  3
identifiable constituent or phase  ).3
 3).
5 2.776 19 2.101
5.2 This te
5.2 test
st met
metho
hod
d ha
hass be
been
en de
desc
scri
ribe
bed
d   (4)   as be
bein
ing
g
6 2.571 20 2.093
7 2.447 21 2.086 superior to other manual methods with regard to effort, bias,
8 2.365 22 2.080 and simplicity.
9 2.306 23 2.074
10 2.262 24 2.069 5.3 Any number of clearly distinguishab
distinguishable
le consti
constituents
tuents or
11 2.228 25 2.064 phases
phases wit
within
hin a micr
microst
ostruc
ructur
turee (or mac
macros
rostru
tructu
cture)
re) can be
12 2.201 26 2.060
13 2.179 27 2.056 counted using the method. Thus, the method can be applied to
14 2.160 28 2.052 any
any ty
type
pe of sosoli
lid
d ma
mate
teri
rial
al frfrom
om wh
whic
ich
h adadeq
equa
uate
te tw
two-
o-
15
16
2.145
2.131
29
30
2.048
2.045
dimensional sections can be prepared and observed.
17 2.120 40 2.020 5.4 A condensed
condensed step-by-st
step-by-step
ep guide for using the method is
18 2.110 60 2.000
given in Annex
in  Annex A1.
A1.
`   1.960

6. Appar
Apparatus
atus
6.1   Test Grid,   consisting of a specified number of equally
spaced points formed by the intersection of very thin lines. Two
PT    = total
total num
number
ber of poi
points
nts in the test gri
grid.
d. common types of grids (circular or square array) are shown in
Pi   = point count on the i th field.
point count
Fig. 1.
1.
PP (i)   =   Pi
3 1005   percen
percentag
tagee of grgrid
id po
poin
ints,
ts, in th
thee 6.1.1 The test grid can be in the form of a transparent
transparent sheet
sheet
P T 
that is super
superimpose
imposed d upon the viewing screen for the measure-
constituent observed on the  i th field.
ment.
n   = numbe
numberr of field fieldss cou
counte
nted.d.
¯  
P̄ p
P   =   1 n 6.1.2   Eyepiece Reticle,  may be used to superimpose a test
n  i(  p
P  ~ i ! 5  arithmetic average of  P  P p   (i). grid upon the image.
5 1
s   = estimate of the stand standard
ard deviati
deviation on (σ) (see (Eq (Eq 3)
in Section 
Section   10 10).
). 6.2   Light
Light Micr
Microscop
oscope,e,   or ot
othe
herr su
suit
itab
able
le de
devi
vice
ce wi
with
th a
95 %   CI = 95 % confi confide denc
ncee inter
interva
vall viewing
viewin g scr
screen
een at leas
leastt 100 mm × 125 125 mm, pre
prefer
ferabl
ably
y wit
with
h
graduated  x  and  y  stage translation controls, should be used to
56 t s / = n ;   see
see Note
 Note 1. 1.
t    = a mul multi
tipl
plieierr rela
relateted
d to the the num
numbeberr of fiel fields
ds image the micro
microstructu
structure.
re.
examined and used in conjunction with the stan- 6.3   Scanning
Scanning Electr
Electron
on Micr
Microscop e,   may
oscope, may al
also
so be usused
ed to
dard deviation of the measurements
measurements to determ determineine image the microstructure; however, relief due to polishing or
the 95% CI. heavy etching must be minimized or bias will be introduced as
V V    = vol
volume
ume fra
fractio
ctionn ofof the
the con
constit
stituen
uentt or
or pha
phasese ex- a res
result
ult of dev
deviati
iation
on fro
from
m a tru
truee two
two-di
-dimen
mensio
sional
nal sect
section
ion
pressed as a percentage (see (Eq ( Eq 5) in Section through the microstructure.
10).
10 ).
6.4   Micrographs,   of properly prepared opaque specimens,
%   RA = % relati
relative
ve accu
accura racy
cy,, a measu
measure re ofof the
the stati
statist
stica
icall
¯   taken with any suitable imaging device, may be used provided
precision = (95 % CI ⁄ P P̄ p  ) × 100.
the fields are selected without bias and in sufficient quantity to
NOTE   1—
1—Table 1  gives the appropriate multiplying factors (t ) for any
Table 1 gives
number of fields measured. properly
prop erly sample the micros
microstructu
tructure.
re.
6.4.
6.4.11 Th
Thee ap
appl
plic
icab
ablele po
poin
intt co
coun
unti
ting
ng gr
grid
id sh
shall
all on
only
ly be
4. Summ
Summary
ary of Test
Test Method applied once to each micrograph. Point counting measurements
should be completed on different fields of view and, therefore,
4.1 A clear plastic
plastic test grid
grid or eyepiece
eyepiece reticle
reticle with a regular
regular
different micrographs. Repeated point count measurements on
array
arra y of tes
testt po
poin
ints
ts is su
supe
peri
rimp
mpososed
ed ov
over
er ththee im
imag
age,
e, or a
an individual micrograph is not allowed.
project
pro jection
ion of the imagimage,
e, pro
produc
duced
ed by a liglight
ht mic
micros
roscop
cope,
e,
6.4.2 The magnification of the micrograph should should be as high
high
scanning
scanni ng electro
electronn micros
microscope,
cope, or microg
micrograph,
raph, and the numb
number
er
as nee
needed
ded to ade
adequa
quately
tely res
resolv
olvee the micr
microst
ostruc
ructur
turee with
without
out
of test points falling within the phase or constituent of interest
resulting in adjacent grid points overlaying a single constituent
are counted and divided by the total number of grid points
feature.
yielding a point fraction, usually expressed as a percentage, for
thatt fiel
tha field.
d. The average
average poi
point
nt fra
fractio
ction
n for   n   measured
measured fields 7. Samp
Sample
le Selection
Selection
gives an estimate of the volume fraction of the constituent. This
method
meth od is app
applica
licable
ble onl
onlyy to bul
bulk
k opa
opaque
que planar sections
sections 7.1
7.1 Sa
Samp
mples
les se
sele
lecte
cted
d foforr me
meas
asur
urem
emenentt of th
thee ph
phas
asee or
viewed with reflected light or electrons. consti
cons titu
tuen
entt sh
shou
ould
ld be re repr
pres
esen
enta
tati
tive
ve of th thee ge
gene
nerarall
microstructure, or of the microstructure at a specified location
5. Sign
Significa
ificance
nce and Use within a lot, heat, or part.

5.1 Thi
Thiss test method
method is bas
based
ed upon the stereolo
stereologic
gical
al pri
prin-
n- 7.2 A descr
description
iption of the sample
sample locations
locations should be
be included
ciple that a grid with a number of regularly arrayed points, as a part of the results.
when
wh en sysyst
stem
emat
atic
ical
ally
ly pl
plac
aced
ed ov
over
er an im
imag
agee of a tw two-
o-
dimensional section through the microstructure, can provide, 3
The boldface numbers in parentheses refer to the list of references at the end of 
after a representative number of placements on different fields, this standard.

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  E562 − 19
TABLE 2 Guidelines for Grid Size Selection A
NOTE   1—A grid siz
sizee sel
select
ection
ion whi
which
ch giv
gives
es a signifi
significan
cantt num
number
ber of 
fields hav
fields having
ing no gri
grid
d poi
points
nts on the constitue
constituent
nt of intere
interest
st sho
should
uld be
avoided.
Visual Area Fraction Estimate
  Grid Size (Numbe
(Numberr of Points
Points,,  P T  )
Expressed as a Percentage
2 to 5 % 100
5 to 10 % 49
10 to 20 % 25
>20 % 16
A
These guidelines represent an optimum for efficiency for the time spent counting
and for the statistical
statistical information obtained
obtained per grid placem
placement.
ent.

8. Sample Preparation
Preparation
8.1 The two-dimension
two-dimensionalal sections should be prepa
prepared
red using
standard
stand ard metallog
metallographi
raphic,
c, ceramo
ceramograph
graphic,
ic, or other polish
polishing
ing
procedures, such as described in Methods E3
Methods  E3..
8.2 Smeari
Smearingng or other distortions
distortions of the phases or constitu-
ents during preparation of the section or sections should be
minimized because they tend to introduce an unknown bias
into the statistical volume fraction estimate.
8.3 Etch
Etching
ing of the sections,
sections, as des
descri
cribed
bed in Test Methods
Methods
Circular Grid E407,, should be as shallow (that is, light) as possible because
E407

deviations
bias towardfrom
overaestimation
planar two-dimensional
of the volumesection will cause a
fraction.
8.4 Stain- or coloring-type
coloring-type etchants
etchants are prefe
preferable
rable to those
that cause attack of one or more of the constituents or phases.
8.5 Descri
Description
ption of the etchant and etching procedure
procedure should
be included in the report.
8.6 If etching is used to provide contrast
contrast or distinguishabil-
distinguishabil-
ity of constituents then the volume fraction estimates should be
obtained as a function of etching time to check the significance
of any bias introduced.

9. Procedur
Proceduree
9.1   Principle:
9.1.1 An array of points
points formed by a grid of lines or curves
is superimposed upon a magnified image (that is, a field of 
view) of a metallographic specimen.
9.1.2 The number of point pointss fallin
falling
g within the microstruc-
microstruc-
tural
tural con
consti
stituen
tuentt of inte
interes
restt is cou
counted
nted and aveaverag
raged
ed for a
selected number of fields.
Square Grid
9.1.3 This average
average number of points expressed
expressed as a percen
percent-t-
NOTE 1—The entire 24 points can be used, or the outer 16, or the inner agee of th
ag thee to
total
tal numbe
numberr of po poin
ints
ts in th
thee ar
arra
ray
y (PT   ) is an
8 points. unbiase
unb iased
d sta
statist
tistical
ical esti
estimati
mation
on of the vol
volume
ume per
percen
centt of the
FIG. 1 Examples of Possible Grid Configurations That Can Be microstructural constituent of interest.
Utilized 9.1.4 A conde
condensed
nsed step-by-ste
step-by-stepp description
description of the proc
procedure
edure
is provided in Annex
in  Annex A1.A1.
9.2   Grid Selection:
7.3 Any orientation
orientation of the prepared
prepared section (that is, whether
whether 9.2.
9.2.11 Th
Thee gr
grid
id sh
shou
ould
ld co
cons
nsis
istt of eq
equa
ually
lly sp
spac
aced
ed po
poin
ints
ts
longitudinal or transverse) can be used. However, it should be form
formeded by ththee in
inter
terse
secti
ction
on of fin
finee lin
lines
es.. Di
Diag
agra
rams
ms of tw
twoo
reco
record
rded
ed sin
since
ce it ma
mayy ha
have
ve an efeffe
fect
ct up
upon
on ththee pr
prec
ecisi
ision
on possible grids, one with a circular pattern and one with a square
obtained. pattern, which are recommended for use, are shown in  Fig. 1. 1.
7.4 If the sample microstructure
microstructure contains
contains gradients or inho- 9.2.2 Determ
Determine
ine the number of points (that
(that is, the grid size,
mogeneities
mogen eities (for example, banding) then the section shou
should
ld PT  ) from a visual estimate of the area fraction occupied by the
contain or show the gradient or inhomogeneity. constituent
const ituent of intere
interest.
st.   Table
Table 2   provides
provides guidelines for this

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  E562 − 19
TABLE 3 Prediction of the Number of Fields (n ) to be Observed as a Function of the Desired Relative Accuracy and of the Estimated
Magnitude of the Volume Fraction of the Constituent
33 % Relative Accuracy 20 % Relative Accuracy 10 % Relative Accuracy
Amount of volume Number of fields n 
fields  n  for
 for a grid of P 
of  P T    = Number of fields  n 
 n  for
 for a grid of P 
of  P T    = Number of fields  n 
 n  for
 for a grid of P 
of  P T    =
fraction,  V v  in percent
fraction, V  16 25 49 100 16 25 49 100 16 25 49 100
points points points points points points points points points points points points
2 110 75 35 20 310 200 105 50 1,250 800 410 200
5 50 30 15 8 125 80 40 20 500 320 165 80
10 25 15 10 4 65 40 20 10 250 160 85 40
20 15 10 5 4 30 20 10 5 125 80 40 20

NOTE   1—The given

  100values in the table above are based on the formula:
n. S  2
4
 E  3 P T 
· DS 2 V v

V V  D
where:
 E    = 0.0.01
01 × % RA
RA,, an
and
d
V V    = is exp
expres
ressed
sed in %.

in  Table 2 do
selection. The values in Table 2  do not correspond
correspond to theor
theoreti-
eti- 9.4.4
cal constraints; but, by using these values, empirical observa- P i 3 100
tions have shown that the method is optimized for a given P P ~i! 5 (1 )
P T 
precision.
9.2.2.
9.2.2.1
1 The user may cho choose
ose to emp
employ
loy a 100 point
point gri
grid
d 9.4.5
9.4.5 Th
Thee va
valu
lues
es of PP(i)   are us
used
ed to ca
calcu
lculat ¯   p   and
latee   P
P̄
over the entire range of volume fractions. The use of 100–point standard deviation,   s.
grid
grid fac
facilit
ilitate
atess eas
easy
y vol
volume
ume per
percen
centt calc
calcula
ulatio
tions.
ns. the use of 
9.5   Selection of the Number of Fields:
onl
only
y one overlay
overlay
determinations may orsave
eyepie
eye piece
ce time
both reticle
reticle
andfor all vol
money. volume
ume percent
percent 9.5.1 The number of fields or images to measure
measure depends on
9.2.2.2
9.2.2.2 For constituents
constituents present
present in amount of less than 2%, the desired degree of precision for the measurement. 
measurement.   Table 3
a 400–point grid may be used. gives a guide to the number of fields or images to be counted
9.2.3 Super
Superimpos
imposee the grid, in the form of a transparency
transparency,, as a function of   PT  , the selected relative accuracy (statistical
upon
upo n a gro
ground
und glass
glass scr
screen
een on whi
whichch the sec
section
tion image
image is precision), and the magnitude of the volume fraction.
projected. 9.6   Selection of the Array of Fields:
9.2.4 A grid
grid in the form of an eyepiece reticle may also be 9.6.1
9.6.1 Use a uniunifor
formly
mly spaced
spaced arr
array
ay of fields to obtobtain
ain the
used. estimated
estimat ed value, P p  , and the estimated standard deviation,   s.
9.2.5
9.2 .5 If the constituen
constituentt are
areas
as for
form
m a reg
regula
ularr or per
period
iodic
ic
9.6.2
9.6.2 If gra
gradie
dients
nts or inh
inhomo
omogen
geneiti
eities
es are pre
presen
sent,
t, the
then
n a
pattern on the section image, avoid the use of a grid having a
unif
un ifor
orm
m sp spaci
acing
ng of fie field
ldss ma
mayy in
intrtrod
oduc
ucee a bibias
as in
into
to th
thee
similar patter
pattern.
n.
estim
estimat
ate.
e. If an
anot
othe
herr met
metho
hodd of fie
fieldld se
selec
lectio
tion
n is us
used
ed,, fo
forr
9.3   Magnification Selection: example, random, then describe it in the report.
9.3.1 Select the magnificatio
magnificationn so that it is as high as needed 9.6.3 When the microstructure
microstructure shows a certain periodicity
periodicity
to clearly resolve the microstructure without causing adjacent of distribution of the constituent or phase being measured, any
grid points to fall over the same constituent feature. coincidence of the points of the grid and the structure must be
9.3.2 As a guide
guideline,
line, choose
choose a magnifi
magnification
cation that gives an avoided.
avoid ed. This can be achieve
achieved d by using either a circular grid or
average constituent size that is approximately one half of the a sq
squa
uarere gr
grid
id pl
plac
aced
ed at an an angl
glee to ththee mi
micr
cros
ostr
truc
uctu
tura
rall
grid spacing. periodicity.
9.3.
9. 3.3
3 As ththee ma
magn
gnifi
ifica
catio
tion
n is in
incr
crea
ease
sed,
d, th
thee fie
field
ld ar
area
ea
decrea
dec reases
ses,, and the field
field-to
-to-fie
-field
ld var
variab
iabilit
ility
y inc
increa
reases
ses,, thu
thuss 9.7  Grid Positioning Over Fields— Make Make grid positioning of 
requiring a greater number of fields to obtain the same degree each field witho
without
ut viewing the micros
microstructu
tructure
re to eliminat
eliminatee any
of measurement precision. possib
pos sibilit
ility
y of ope
operato
ratorr bia
bias.
s. Thi
Thiss can be acco
accompl
mplish
ished
ed by
moving the   x   and   y   stage mechanism a fixed amount while
9.4   Counting:
shifting to the next field without looking at the microstructure.
9.4.1 Count and record
record for each field the numbe
numberr of points
falling on the constituent of interest. 9.8   Improving Measurement Precision— It It is recommended
9.4.2 Count any points falling on the constituent boundary
boundary thatt the user atte
tha attempt
mpt to samp
sample
le mor
moree of the microstru
microstructu
cture
re
as one half. either by multiple specimens or by completely repeating the
9.4.3 In order to minimize
minimize bias, any point
point that is doubtful as metallo
met allogra
graphi
phicc pre
prepar
paratio
ation
n on the sam
samee sam
sample
ple whe
whenn the
to whether it is inside or outside of the constituent boundary precision for a single set of data is not acceptable (see Section
should be counted as one half. 11).
11).

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  E562 − 19

10. Calculation of the Volume

Volume Percentage
Percentage Estimate and accuracy, % RA, should be calculated using the increased total
% Relative Accuracy number of fields as a single data set.
10.1 The average percentage
percentage of grid points on the features 11.
1.5
5 If ad
addi
ditio
tiona
nall sesecti
ction
onss ar
aree pr
prep
epar
ared
ed fr
from
om th
thee sa
same
me
of int
interes
erestt pro
provid
vides
es an unb unbias
iased
ed stat
statist
istical
ical esti
estimato
matorr for the sample by completely repeating the sample preparation, or if 
volume percentage within the three dimensional microstruc- additio
add itional
nal sam
sample
pless are preprepar
pared,
ed, the
thenn the sam
samee pro
proced
cedure
ure
ture. The value of the multiplier,   t , can be found in  Table 1. 1. should be used for each section, and the data recorded and
Thus, the average,  P ¯ 
 
 P̄ p  , the standard deviation estimator,  s , and report
reported
ed sep
separa
arately
tely.. A gra
grand
nd ave
averag
ragee can be calc
calculat
ulated
ed by
the 95 % confidence interval, 95 % CI, should be calculated taking the average of the set means in this case. If no sample
and recorded for each set of fields. The equations for calculat- hetero
heterogen
geneity
eity is ind
indicat
icated
ed (th
(that
at is, the con
confide
fidence
nce inte
interva
rvals
ls
ing these values are as follows: about the mean of each set overlap), then the 95 % CI can be
n calculated from the standard deviation obtained using the data
¯     5 1
P
P̄  p
n   ( P  ~ i !
i 1
 p   (2 ) from all of the sets (that is, pooling the data and calculating a
5

mean, standard deviation, and 95 % CI).

1/ 2

F
n

s5
  1
n21  ( @ P
i 5 1
¯    # 2
 p  ~ i ! 2 P
P̄  p G (3 ) 11.6 Where the 95 % CI do not overlap for
then a statistic
statistically
ally significant differenc
for the different
differencee betwee
between
different sets,
n sample
sampless or
s sections may be present. In this case, more rigorous statistical
95% CI 5 t  3 (4 )
=n significance tests should be considered.

10.2 The volume percentage

percentage estimate
estimate is given as: 12. Repo
Report
rt
¯  
V v   5 P
P̄ 6 95 % CI (5)
 p 12.1 Report the following information:
information:
10.3 An estimate of the % relative accuracy
accuracy associated
associated with 12.1.1
12. 1.1 Raw data; note when   n   > 30, the reporting of raw
the estimate can be obtained as: data is optional, however, the raw data shall be available for
review when requested,
95% CI ¯   p  ) 6 95 % CI,
% RA 5 3 100 (6) 12.1.2
12.1. 2 Estimate
Estimatedd volume % (P P̄
P̄
P
¯   p 12.1.3
12.1. 3 Standa
Standard
rd deviation,
12.1.4
12.1. 4 % relative accuracy (calculated
(calculated value, not one esti-
10.3.1 Estimat
Estimates
es for the number of fields required
required to obtain
mated from Table
from  Table 2),
2),
a % relative accuracy of 10, 20, or 33 % with different volume
12.1.5
12.1. 5 Numbe
Numberr of fields per metallographic
metallographic section,
section,
percen
percentag
tages
es and gri
grid
d siz
sizes
es are pro
provid
vided
ed in   Table
Table 3. The
These
se
12.1.6
12.1. 6 Numbe
Numberr of sections,
values were calculated under the assumption that the features
12.1.
12 .1.7
7 Sam
Sample
ple des
descri
cripti
ption
on and pr prepa
eparat
ration
ion,, inc
includ
luding
ing
have a random distribution upon the metallographic section.
etchant, if used,
10.4 The % rel
10.4 relativ
ativee acc
accura
uracy
cy rep
report
orted
ed sho
should
uld   always   be 12.1.8
12.1. 8 Section orientation,
orientation,
calculated from the sample data and should not be taken from 12.1.9
12.1. 9 Magni
Magnification
fication,,
Table 3.
3. 12.1.10
12.1. 10 Grid description,
description,
12.1.11
12.1. 11 Field array description
description and spacin
spacing,
g, and
11. Improving the Volume
Volume Fraction Estimate 12.1.12
12.1. 12 List of volume % estimates for each metallograp
metallographic
hic
section 6 95 % CI.
11.
1.1
1 If ad
addi
ditio
tiona
nall fie
field
ldss ar
aree me
meas
asur
ured
ed to re
redu
duce
ce th
thee %
relative accuracy, then the following rule gives an excellent
13. Ef
Effort
fort Required
Required
guideline: To reduce the % RA by 50 %, then a total of four 13.1 A reasonable
reasonable estimate
estimate for the time requi
required
red to perform
times the original number of fields should be measured.
thee ma
th manu
nual
al po
poin
intt co
coun
untt on 30 fiefield
ldss fo
forr a sin
singl
glee ty
type
pe of 
11.
1.2
2 When
When ad addi
ditio
tiona
nall fie
fields
lds araree sel
select
ected
ed on th thee sam
samee micr
mi cros
ostru
tructu
ctura
rall fe
feat
atur
uree is 30 mi
min.n. Th
Thisis ti
time
me es
estim
timat
atee ca
can
n
secti
section
on,, th
they
ey sh
shou
ould
ld nonott ov
over
erlap
lap th
thee in
init
itial
ial se
sett bu
butt ma
mayy fit
probably be decreased to 15 min after some experience and
betw
be twee
een
n fie
field
ldss of th
thee in
init
itia
iall se
set,
t, an
andd sh
shou
ould
ld al
also
so fo
form
rm a familiarity with the point counting procedure and the micro-
systematic sampling array. structure analyzed are obtained.
11.3
11 .3 As an example,
example, if a 6 by 5 arr array
ay of fields was used
used to
obtain the initial set, then by halving the spacing and measur- 14. Pre
Precision and Bias4
cision
ing the intermediate field positions, a total of four times the 14.1
14 .1 The sy
syste
stema
matic
tic po
poin
intt co
coun
untt tec
techn
hniq
ique
ue is th
thee mo
mostst
number
num ber of fiel
fields
ds can be mea measur
sured.
ed. Hence,
Hence, 120 total fields efficient manual techni
eff technique
que for development
development of an unbia
unbiased
sed
would be measured by halving the spacing (in both   x   and   y estimate of the volume fraction of an identifiable constituent or
directions)
directions) and measur
measuringing the interm
intermediate
ediate positions
positions to form a phase.
12 by 10 ar arra
ray
y. Th
Thisis ad
addi
ditio
tiona
nall ef
effo
fort
rt sh
shou
ould
ld re
redu
duce
ce th
thee
14.2
14.2 The pre
presen
sence
ce of per
period
iodicit
icity
y, str
struct
uctura
urall gra
gradie
dients
nts or
confide
con fidence
nce inte
interva
rval,
l, and thu
thuss the % RA, by app approx
roximat
imately
ely
inhomogeneities in the section can influence the precision and
50 %.
11.
1.4
4 Wh
Wher
eree ad
addi
ditio
tiona nall fiefield
ldss ar
aree me
measu
asure
red
d on th
thee sa
same
me
 P̄¯   p  , the standard deviation estimate,  s, the
section, the average,  P 4
Supporting data have been filed at ASTM International Headquarters and may
95 % co confi
nfide
denc
ncee in
inte
terv rvalal,, 95 % CI CI,, an
and
d th
thee % rerela
lati
tive
ve be obtained by requesting Research Report RR:E04-1003.

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  E562 − 19
TABLE 4 Results of Interlaboratory Point Counting Round-Robin 5

¯ p  (%)   Repeatability Reproducibility Repeatability Reproducibility Repeatability Reproducibility

Micrograph   P 
Std. Dev. (%) Std. Dev. (%) 95 % CI (%) 95 % CI (%) % RA % RA
25 Point Test Grid
A 9.9 5.3 5.3 14.8 14.8 149.5 149.5
B 17.8 6.6 6.9 18.6 19.4 104.5 109.0
C 27.0 8.8 9.4 24.7 26.2 91.5 97.0
100 Point Test Grid
A 9.3 3.9 3.9 11.0 11.0 118.3 118.3
B 15.9 3.4 4.0 9.4 11.2 59.1 70.4
C 25.1 3.9 4.3 10.9 12.1 43.4 48.2

accuracy
accura cy of the volume fraction estimate. Guidelines are given 14.9 If a greater degree of precision
precision and relative
relative accuracy
accuracy is
in   7.4
in 7.4,,  9.2.5
 9.2.5,,  9.6.2
 9.6.2,,  9.6.3
 9.6.3,,  11.5
 11.5   and
and 11.6
 11.6.. required, follow the guidelines in Section 
Section   11
11..
14.3 The qua
14.3 quality
lity of the sam
sample
ple pre
prepar
paratio
ation
n can infl
influen
uence
ce 14.10 Results from a roun round-rob
d-robin
in interla
interlaborat
boratory
ory program
precision and accuracy of the volume fraction estimate. Guide- (5),  where three micrographs with different constituent volume
), where
lines are given in Section  8
 8.. fractions were point counted using two different grids (25 and
14.4 The point density
density of the grid used to make the volume 100 poipoints
nts)) by 33 dif differ
ferent
ent ope
operato
rators,
rs, wer
weree ana
analyz ed4 in
lyzed
fraction estimate can influen
fraction influencece the ef
effficiency
iciency,, precis
precision
ion and accordance
accord ance with Practic
Practicee   E691   to devel
developop repeat
repeatability
ability and
relative accuracy of the volume fraction estimate. Guidelines reproducibility standard deviations and 95 % confidence limits
are given in 9.2
in  9.2.. (see Table
(see  Table 4).
4). For the same number of random grid placements
14.5 The magnificati
14.5 magnification
on emp
employ
loyed
ed in the poi
point
nt cou
count
nt can (10) on each micrograph, the repeatability and reproducibility
influence precision and relative accuracy. Guidelines are given standard
stand ard devia
deviations
tions and 95 % confid confidence
ence interv
intervals
als increa
increased
sed
in   9.3
in 9.3.. with increasing  P ¯ 
 
 P̄ p for measurements with the 25 point test grid
14.6 The counting
counting of grid points at a consti
constituent
tuent boundary
boundary,, but were essentially constant for the 100 point test grid. Note

particu
particular
larly
ly wh
when
en do
doub
ubtt ex
exis
ists
ts as to th their
eir ex
exact
act lo
loca
catio
tion,
n, that the interlaboratory % relative accuracies (which are much ¯   p
presents an opportunity for bias in the estimate of the volume poorer than those for the individual operators) improve as   P P̄
fraction. Guidelines are given in  9.4.2
 9.4.2,, and 9.4.3
and  9.4.3.. increases and as the grid point density (PT  ) increa
increases.
ses. The 100
point grid, with four times the number of grid points, decreased
14.7
14. 7 The number
number of fiel fields
ds measured,
measured, the met
method
hod of field
the relative accuracies by about 21 to 51 % as   P ¯   p   increased
P̄
selection
selection and thetheir
ir spa
spacin
cingg wil
willl infl
influen
uence
ce the pre
precis
cision
ion and
relative accuracy of the volume fraction estimate. Guidelines (Micrographs A to C).
are given in 9.5
in  9.5,, and 
and   9.6
9.6..
14.8 The precision
precision of a given measurement
measurement of the volum
volumee
fraction is determined by calculation of the standard deviation,
95 % confidence interval, and % relative accuracy as described
in Section 
Section   10
10..

ANNEX

(Mandatory Information)

A1. PROCEDURE
PROCEDURE FOR SYST
SYSTEMA
EMATIC
TIC MANU
MANUAL
AL POIN
POINT
T COUN
COUNT
T

A1.1 Visually estimate area percent of constituent

constituent or feature 95% CI
% RA 5 3 100
of interest on metallographic section. ¯  
P̄
P p

A1.2 Using Table
Using  Table 3,
3, select grid size,  P T  . A1.5 Using   Table 3, 3, obtain an estimate of the number of 
A1.3 Super
Superimpos
imposee the grid upon the microscope viewing fields,   n, required to obtain the desired degree of precision.
screen
screen an
and
d sel
selec
ectt ma
magn
gnifi
ificat
catio
ion
n su
such
ch th
that
at th
thee si
size
ze of th
thee NOTE   A1.1—A minimum of 30 fields must be measured in order to
features of interest are approximately one half of the spacing calculate the 95 % confid
calculate confidence
ence interval using the equation given in  A1.12
 A1.12..
between grid points. A1.6 Determi
Determine
ne the spacing between fields
fields that will form a
A1.4 Select a statistical precision
precision,, (% RA) for example, 10, systematic (equally spaced) array covering a majority of the
20, or 33 %, desired for the measurement. Note that the % RA sample area without overlap.
is defined as follows:

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  E562 − 19

A1.
A1.6.1
6.1 For example
example,, on a 10 mm × 15 mm spe specime
cimenn are
areaa NOTE A1.3—A hand calculator with a  ∑
 ∑ +
 + key can be used to calculate
where 40 fields are indicated from  Table 3,
3, a 5 by 8 array of  these quantities.
fields at 1.5 mm intervals might be used. A1.10 The average percentage
percentage of points is:
A1.7 Determ
Determine
ine the number of turns required on the stage n n
¯     5 1 1
translation knobs to move the stage from one field position to P
P̄  p
n  (
i 5 1
P p  ~ i ! 5
n  ( P  / P
i 5 1
i T    3 100

the next. Do not observe the image while translating to a new

field to avoid bias in positioning the grid. A1.11
A1.11 The standard deviation
deviation estimate is:
n 1/ 2
A1.8 Count and record
record the number of grid points,
points, Pi , falling   1
s5 @ P p ~ i ! 2 PP̄¯   p # 2
5
1
n21
within the features of interest.
F  (
i

NOTE A1.2—Any point that falls on the boundary should be counted as

one half. To avoid bias, questionable points should be counted as one half. A1.12 The 95 % confidence  P̄¯   p  is:
confidence interval for P
G
A1.9 Calcula
Calculate
te the average
average % of points per field,
field,  P¯   p , and its
 P̄ ts
95% CI 5
standard deviation,   s. =n

REFERENCES

(1)   DeHof
DeHoff,f, R. T., and Rhi
Rhines
nes,, F. N.
N.,, eds .,   Quantitative Microscopy,
eds., (4)   Hilliard
Hilliard,, J. E., and Cah
Cahn,
n, J. W.,
W., “An Evaluatio
Evaluationn of Pro
Proced
cedure
uress in
McGraw-Hill Book Co., New York, NY, 1968. Quantitative Metallography for Volume-Fraction Analysis,”  Transac-
(2)  Underwood, E. E.,  Quantitative Stereology, Addison-Wesley Publish- tions AIME , Vol 221, 1961, pp. 344–352.
ing Co., Reading, MA, 1970. (5)   Abrams, H., “Practical Applications of Quantitative Metallography,”
(3)   Howard
Howard,, R. T., and Coh
Cohen,
en, M., “Qu “Quant
antita
itative
tive Met
Metall
allogr
ograph
aphy
y by Stereology and Quantitative Metallography, ASTM STP 504 , ASTM,
Point-Counti
Point-Counting
ng and Lineal Analysis,”
Analysis,”   Transactions AIME , Vol 172, Philadelphia, PA, 1972, pp. 138–182.
1947, pp. 413–426.

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