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INTRODUCTION
This practice may be used to produce stereological measurements that describe the amount, number,
size, and spacing of the indigenous
indigenous inclusions (sulfides
(sulfides and oxides) in steels. The method may also be
applied to assess inclusions in other metals or to assess any discrete second-phase constituent in any
material.
1. Sco
Scope
pe 2. Referenc
Referenced
ed Documents
1.1 This practice
practice describes a procedure for obtaining
obtaining stereo- 2.1 ASTM Standards:2
logical measurements
measurements that descri
describe
be basic characteristics
characteristics of the E 3 Guide for Preparation of Metallographic Specimens
morphology of indigenous inclusions in steels and other metals E 7 Terminology Relating to Metallography
using automatic image analysis. The practice can be applied to E 45 Test Methods for Determining the Inclusion Content
provide such data for any discrete second phase. of Steel
E 768 Guide for Prepa
Preparing
ring and Evalua
Evaluating
ting Specimens for
NOTE 1—Stereological measurement methods are used in this practice
to assess the average characteristics of inclusions or other second-phase Automatic Inclusion Assessment of Steel
particles
particl es on a longi
longitudina
tudinall plane-
plane-of-po
of-polish.
lish. This infor
information
mation,, by itself
itself,,
does not produ
produce
ce a three-
three-dimen
dimensiona
sionall descri
description
ption of these constituents
constituents in
3. Terminology
space as defor
deformatio
mationn proce
processes
sses cause rotation and alignm
alignment
ent of these 3.1 Definitions:
constituents
consti tuents in a prefer
preferred
red manner.
manner. Develo
Developmen
pmentt of such information
information 3.1.
3.1.11 Fo
Forr de
defin
finiti
ition
onss of ter
terms
ms us
used
ed in th
this
is pr
prac
actic
tice,
e, see
requires measurements on three orthogonal planes and is beyond the scope Terminology E 7.
7.
of this practice.
3.2 Symbols:
1.2 Th
1.2 This
is pr
prac
actic
ticee sp
speci
ecific
ficall
ally
y ad
addr
dres
esse
sess th
thee pr
prob
oblem
lem of
producing
produ cing stereological
stereological data when the features of the constitu-
¯
A
Ā = the averag
averagee area of inclus
inclusions
ions or particl es, µm 2 .
particles,
ents to be measured make attainment of statistically reliable
data difficult. A A = the area fractio
fraction
n of the inclus
inclusion
ion or consti
constituent.
tuent.
1.3 This prapractic
cticee dea
deals
ls onl
only
y wit
with
h the rec
recomm
ommend
ended
ed test Ai = the are
areaa of the det
detecte
ectedd feat
feature
ure..
AT = the mea
measursureme
ement
nt are
areaa (fie
(fieldld are a, mm2).
area,
methods and nothing in it should be construed as defining or
H = the tota
totall projec
projected
ted len
length
gth in the
the hot
hot-wo
-worki
rking
ng
establishing limits of accepta
establishing acceptability
bility.. T
direction of the inclusion or constituent in the
1.4
1.4 ThThee va
valu
lues
es sta
state
ted
d in SI ununitsits are to be re rega
gard
rded
ed as
field, µm.
standard. No other units of measurement are included in this
L¯
L̄ = the averag
averagee length in the hot-w
hot-workin
orkingg direct
direction
ion
standard.
of the inclusion or constituent, µm.
1.5 This standar
standard d doe
doess not purport
purport to add addreress
ss all of the LT = the true length of scan lines, pixel lines, or grid
safet
sa fetyy co
conc
ncer
erns
ns,, if an
anyy, as
asso
socia
ciated
ted wi with
th it
itss us
use.
e. It is th
thee lines (number of lines times the length of the
responsibility of the user of this standard to establish appro- lines divided by the magnification), mm.
priate safety and health practices and determine the applica- n = the numbe
numberr of fields measur
measured.ed.
bility of regulatory limitations prior to use.
1
This practice is under the jurisd
jurisdictio
iction
n of ASTM Committee
Committee E04 on Metal
Metallog-
log-
2
raphy and is the direct responsibility
responsibility of Subc
Subcommitte
ommitteee E04.1
E04.14
4 on Quanti
Quantitativ
tativee For refere
referenced
nced ASTM stand
standards,
ards, visit the ASTM webs
website,
ite, www
www.ast
.astm.org
m.org,, or
Metallography. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current
Current editio
edition
n approv
approved
ed Oct. 1, 2008. Publi
Published
shed January 2009. Originally Standards volume information, refer to the standard’s Document Summary page on
approved in 1988. Last previous edition approved in 2003 as E 1245 – 03. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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E 1245 – 03 (2008)
5. Sign
Significan
ificance
ce and Use 6. Interfere
Interferences
nces
5.1 This practice
practice is used to assess the indigenous
indigenous inclusions
inclusions 6.1 Void
Voidss in the metal due to sol solidi
idifica
fication
tion,, limi
limited
ted hot
or second-phase constituents of metals using basic stereologi- ductility, or improper hot working practices may be detected as
cal procedures performed by automatic image analyzers. oxid
ox ides
es be
becau
cause
se th
thei
eirr gr
gray
ay le
leve
vell ra
rang
ngee is sisimil
milar
ar to th
that
at of
5.2 This practice
practice is not suitable for assessing
assessing the exogenous
exogenous oxides.
inclusions in steels and other metals. Because of the sporadic, 6.2 Exoge
Exogenous
nous inclusions,
inclusions, if presen
presentt on the plane-
plane-of-po
of-polish,
lish,
unpredictab
unpre dictable
le natur
naturee of the distri
distribution
bution of exoge
exogenous
nous inclu- will be detected as oxides and will bias the measurements of
sions, other methods involving complete inspection,
inspection, for ex- the indigenous oxides. Procedures for handling this situation
ample, ultrasonics, must be used to locate their presence. The are given in 12.5.9
in 12.5.9..
exact nature of the exogenous material can then be determined 6.3 Imp
Improp
roper
er pol
polish
ishing
ing tech
techniq
niques
ues tha
thatt leav
leavee exc
excessi
essivel
vely
y
by sesecti
ction
onin
ing
g in
into
to th
thee su
susp
spect
ect re
regi
gion
on fofollo
llowe
wedd by seseri
rial,
al, large scratches on the surface, or create voids in or around
step-wise grinding to expose the exogenous matter for identi-
3 4
Vander Voort,
Voort, G. F., “Image Analysis,”
Analysis,” Vol
Vol 10, 9th ed., Metals Handbook: Underwood, E. E., Quantitative Stereology, Addison-Wesley Publishing Co.,
Materials Characterization, ASM, Metals Park, OH, 1986, pp. 309–322. Reading, MA, 1970.
--`,`,,`,,,```,````,,,,``,-`-`,,`,,`,`,,`---
E 1245 – 03 (2008)
inclusions, or remove part or all of the inclusions, or dissolve interior billet locations will be more representative of the bulk
water-soluble inclusions, or create excessive relief will bias the of the material. Additionally, the inclusion content will vary
measurement results. with the ingot pouring sequence and sampling should test at
6.4 Dust, pieces
pieces of tissue paper,
paper, oil or water stains, or other least the first, middle and last ingot teemed. The same trends
foreign
foreign debris
debris on the sursurfac
facee to be examined
examined wilwilll bia
biass the are observed in contin
continuousl
uouslyy cast steels. Samplin
Sampling
g scheme
schemess
measurement results. must be guided by sound engineering judgment, the specific
6.5 If the programming
programming of the movemmovement
ent of the automa
automatictic processing parameters, and producer-purchaser agreements.
stage is improper so that the specimen moves out from under
the objective causing detection of the mount or air (unmounted 9. Test Specimens
specimen),
6.6 Vibr measurements
ibratio
ations mustt be will
ns mus be
elimina
elim biased.
inated
ted if they cause motion
motion in 9.1 In general,
general, test specimen orientation
orientation within the test lot is
the same as described in Practice E 45 45 (Microscopical Meth-
the image.
ods). The plane-of-polish should be parallel to the hot-working
6.7 Dust in the microscope or camera system may produce
produce
axiss and
axi and,, mos
mostt com
common
monly ly,, tak
taken
en at the qua quarte
rter-
r-thi
thickn
ckness
ess
spurious indications that may be detected as inclusions. Con-
locatio
loc ation.
n. Oth
Other
er test locations
locations may also be sam sampled
pled,, for ex-
sequently, the imaging system must be kept clean.
ample, subsurface
subsurface and center locations, as desir desired
ed or required.
7. Appar
Apparatus
atus 9.2 The surface
surface to be polished
polished should
should be large enough
enough in
7.1 A reflected light microscope
microscope equipped with bright-field
bright-field area
area to pe perm
rmit
it me
meas
asur
urem
emenentt of at le leas
astt 10
1000 fie
field
ldss at ththee
objectives
objecti ves of sui suitabl
tablee mag
magnifi
nificati
cations
ons is useusedd to ima
imagege the necessary
necess ary magnification.
magnification. Larg Largerer surfac
surfacee areas are benefi
beneficial
cial
microstructure. The use of upright-type microscope allows for whenev
whe never
er the proproduc
ductt for
formm perpermits
mits.. A min
minimu
imumm polpolish
ished
ed
easier stage control when selecting field areas; however, the surface area of 160 mm 2 is preferred.
specimens will require leveling which can create artifacts, such 9.3 Thin product
product forms can be sampled
sampled by placing a number
number
as scr
scratc
atche
hes,
s, du
dust
st re
remn
mnan ants
ts an
andd st
stain
ainin
ing,
g, on th thee po
polis
lishe
hed
d of lo
long
ngitu
itudi
dina
nally
lly or
orie
ient
nted
ed pipiece
ecess in ththee mo
moun
untt so ththat
at th
thee
surface (see 12.2.1
(see 12.2.1). ). The use of inverted microscopes usually sampling area is sufficient.
result
res ult in a mor moree conconsist
sistent
ent foc
focus
us bet
betwee
ween n field
fields,s, the
thereb
rebyy, 9.4 Practic
Practicee E 768 lists
768 lists two accepted methods for prepar preparing
ing
requ
re quiri
iring
ng les
lesss fofocu
cuss
ssin
ingg be
betw
tween
een fiel
fields
ds an
andd a mo morere rarapi
pid
d steel samples for the examination of inclusion content using
completion of the procedure. A scanning electron microscope image analysis. The standard also lists a procedure to test the
also may be used to image the structure. quality of the preparation using differential interference con-
7.2 A programmabl
programmablee automa automatic
tic stage to control movement trast (DIC)
(DIC)..
in the x and y directions without operator attention is recom-
mended (but not mandatory) to prevent bias in field selection 10. Specimen Preparation
Preparation
and to minimize operator fatigue. 10.1 Metallographic specimen preparation must be carefully
7.3 An automatic
automatic focus device device may also be employedemployed if controlled to produ
controlled produce
ce accepta
acceptable
ble quality surfa
surfaces
ces for image
found
fou nd to be rel reliab
iable.
le. Suc
Such h dev
devices
ices may be unr unrelia
eliable
ble when analysis. Guidelines and recommended practices are given in
testing steels or metals with very low inclusion contents. Methods E
Methods E 3, and Practices E
Practices E 45 and E 768.
768.
7.4 An automatic
automatic image analyzer
analyzer with a camera of adequate
10.2 The polishing
polishing procedure
procedure must not alter the true appear-
appear-
sensit
sen sitiv
ivity
ity is empemplo loye
yed d to dedete
tect
ct th
thee in
inclu
clusio
sions
ns,, pe
perf
rfor
orm
m
ancee of the inc
anc inclus
lusion
ionss on the plan
plane-o
e-of-p
f-poli
olish
sh by pro
produc
ducing
ing
-
-
`
,
discriminatio
discrim ination,
`
,
, n, and make measurmeasurements.
ements.
`
,
, exces
ex cessiv
sivee rel
relief
ief,, pi
pitti
tting
ng,, cr
crack
acking
ing or pupullo
llout.
ut. Mi
Mino
norr fin
finee
7.5 A compute
,
`
` computerr is use used d to sto
store
re and anaanalyz
lyzee the measure-
measure-
scra
scratch
tches,
es, su
such
ch as frfrom
om a 1-1-µm
µm di
diam
amon
ondd ababra
rasiv
sive,
e, do no
nott
`
,
`
ment data.
`
`
`
,
,
,
,
7.6
7.6 A pr
`
`
, prin
inte
terr is ususeded to ououtp
tput
ut ththee da
data
ta an
andd rerele
leva
vant
nt usually interfere with inclusion detection but heavier scratches
-
`
- are to be avoided. Proper cleaning of the specimen is necessary.
identification/background information in a convenient format.
`
,
,
Use of aut
automa
omatictic gri
grindi
nding
ng and pol
polish
ishing
ing dev
devices
ices is rec
recom-
om-
`
,
,
`
E 1245 – 03 (2008)
10.6
10. 6 The polpolish
ished
ed sur
surfac
facee area for mou mounte
ntedd spe
specime
cimensns 12.1.4 Adj
12.1.4 Adjust
ust the mag
magnifi
nificati
cation
on of the sys
system
tem to pro
provid
videe
should be somewhat greater than the area required for mea- adequate resolution of the inclusions with the largest possible
surement to avoid edge interferences. Unmounted specimens field size. Choice of the optimum magnification is a compro-
gene
ge nera
rally
lly sh
shou
ould
ld ha
have
ve a su surf
rface
ace ararea
ea mu
much
ch grgrea
eater
ter th
than
an mise between resolution and field-to-field measurement vari-
requ
require
iredd fo
forr me
meas
asur
urem
emen
entt to fa
faci
cilit
litat
atee lev
leveli
eling
ng ususin
ing
g ththee ability. Higher magnification objectives have higher numerical
procedure
proced ure descri
described
bed in
in 12.1.1
12.1.1.. aperture ratings and provide improved resolution. However, as
10.7
10 .7 Etchin
Etchingg of sp
spec
ecime
imensns is no
nott dedesi
sire
red
d fo
forr in
incl
clus
usio
ionn magnification
magnifi cation increases, the field-
field-to-fiel
to-field
d measur
measurement
ement vari-
assessment. ability increases,
increases, which increases
increases the standard deviation of the
measurement.
measur ement. Also,
Also, as the magnification
magnification increas
increases,
es, the field
11. Calibration and Standardization
Standardization
11.1 Use a stag
stagee mic
microm
rometer
eter to dete
determi
rmine
ne the size of the area decreases.
four times For fields
as many example,
mustifbethe magnification
measured to coveris the
doubled,
same
frame
frame to cali
calibra
brate
te the image anaanalyz
lyzer
er and to detdeterm
ermine
ine the test area. In general, the lower the inclusion content, the higher
overall magnification of the system for each objective. the required magnification, and vice-versa. Intermediate mag-
11.2 Follow the manufacturer’s recommendations in adjust- nification
nificati on object
objectives
ives (for exampl
example,e, 323, 403, 503, 603, and -
-
-
ing the microscope light source and setting the correct level of 803) provide the best combination of resolution and field area.
`
,
,
`
,
`
Avoi
voidd use of lowlower
er mag
magnifi
nificat
cation
ion obj
objecti
ectives
ves tha
thatt wil
willl not ,
`
,
,
`
-
mende
men ded
d to esesta
tabl
blish
ish th
thee co
corr
rrec
ectt se
setti
tting
ng of ththee gr
gray
ay-l
-lev
evel
el recommended that the same objective be used for all measure- ,
`
`
`
,
,
level histogram of the microstructure can be used to define the example, 323 to 503 objectiv
`
gray
gra y lev
level
el ran
range
ge and threshold
threshold set
setting
tingss for the inc
inclus
lusion
ion or amounts of inclusions, such as free-machining grades, and 50 3
constituent types (see 12.2.1
(see 12.2.1).
). These settings are verified by the to 803 objecti
objectives
ves for vacvacuum
uum deg degass
assed,
ed, ladl
ladle-r
e-refin
efined,
ed, or
flicker method. double-melt grades.
12. Procedur
Proceduree 12.1.5
sou rce forSelect
source bestt the
bes optimum
resolu
resolutio n. Ifmagnification
tion. necessa
necessary andble
ry,, ena
enable adjust
the the light
shadin
shadingg
12.1 Setting Up the Microscope: correction
corre ction adjust
adjustment
ment for chose
chosenn object
objective.
ive.
12.1.1
12.1. 1 Place the specimen on the microscopemicroscope stage so that
12.2 Setting the Densitometer :
the specimen surface is perpendicular to the optic axis. With an
inverted-type microscope, simply place the polished face down 12.2.1
12.2. 1 Gray-
Gray-level
level threshold
threshold settings are selecte
selected d to permit
on the stage plate and hold it in place with the stage clamps. indepe
ind epende
ndent
nt det
detecti
ection
on of sulsulfide
fidess and oxi
oxides
des,, or a spe
specific
cific
With an upright-type microscope, place the specimen on a slide discrete
discre te second phase, using the “flicke
“flickerr method
method”” of switching
and level the sur surfac
facee usi
using
ng cla
clay
y or pla
plastic
sticene
ene bet
betwee
ween n the back and forth between the inclusion image and the thresh-
spec
sp ecime
imen n an
andd sl
slid
ide.
e. If tis
tissu
suee pa
pape
perr is pl
plac
aced
ed be
betwe
tween
en th
thee olded image. The threshold
threshold limits are set for the oxides and the
specime
spe cimen n sur
surfac
facee and the ram of the levelingleveling prepress,
ss, small sulfides so that the inclusions are detected without enlargement
piece
piecess of tistissu
suee pa
pape
perr mamayy ad
adhe
here
re to th thee su
surf
rface
ace duduri
ring
ng of th
thee lar
large
gerr in
inclu
clusi
sion
ons.
s. In so
some
me in
inst
stan
ance
ces,
s, ththee th
thre
resh
shol
old
d
flattening and produce artifacts that affect measurements. In settings may require a minor compromise between detection of
some
so me cascases
es,, ad
adhe
here
rent
nt tis
tissu
suee pa
pape
perr ca
can
n be bl blow
ownn of
offf th
thee the smallest inclusions and overdetection of the largest inclu-
specimen surface. An alternative leveling procedure to avoid sions. The chosen threshold settings should be tried on inclu-
this problem is to place an aluminum or stainless steel ring sions in a number of fields before beginning the analysis. The
form of appropriate diameter, that has been flattened slightly in threshold
thresh old range for oxides
oxides is clo
close
se to the black end of the
a vise to an oval shape, between the specimen and the ram. If reflecta
refl ectance
nce sca
scale
le whi
while
le the ran
range
ge for sulfides
sulfides is som
somewh
ewhat
at
the specimen was mounted, the ring form will rest only on the higher. An alternate approach to establish the threshold settings
surface of the mount. If the specimen is unmounted but with a is to develop a gray-level reflectance histogram of the inclusion
surface area substantially greater than required for measure- or constituent types present, as well as the matrix (usually in
ment, the ring form can rest on the outer edges of the specimen the as-polished condition). The histogram is used to identify
during leveling and thus not affect the measurement area. Some the start (darkest gray) and end (lighte
(lightest
st gray) of the gray level
upright-type microscopes can be equipped with an autoleveling range for each inclusion or constituent type and the intersection
stage for mounted specimens. gray level for two inclusions or constituent types with over-
12.1.2
12.1. 2 For an image analyzer that uses the TV-raste TV-rasterr lines to lapping gray level ranges. Verify these settings by use of the
make intercept counts, align the specimen on the stage so that flicker method for several randomly selected fields.
the longitudinal direction is parallel to the y direction of the 12.2.2
12.2. 2 For steels with very low inclusion contents
contents and very
stage and the inclusions are oriented vertically on the monitor small inclusions, it may not be possible to reliably separate
screen. For a software-based system, the longitudinal direction oxid
ox ides
es fr
from
om su
sulfi
lfide
des.
s. In su
such
ch cas
cases
es,, de
detec
tectt all in
inclu
clusi
sion
onss
of the specimen may be oriented parallel to either the x or y without attempting a separation. For other metals containing
axis of the stage. inclusions of one or more types, adjust the threshold settings to
12.1.3
12.1. 3 The microscope
microscope light source should be checked for sepa
separa
rate
te ththem
em by ty
type
pe or co
colle
llecti
ctive
vely
ly as rerequ
quir
ired
ed by ththee
correc
cor rectt alig
alignme
nmentnt and the illu illumin
minatio
ationn inte
intensi
nsity
ty sho
should
uld be particular application.
adjusted to the level required by the television scanner tube. 12.3 Stage Movement :
E 1245 – 03 (2008)
12.3.1
12.3.1 The stage controls
controls are set to move the specimen
specimen in a 12.5.4
12.5. 4 With an image analyzer that utilizes the raster lines
square or rectangular pattern without running off the specimen for intercept
intercept cou
counti
nting,
ng, for each fiel
field,
d, cou
count
nt the num
number
ber of
surface. Depending on the area of the plane-of-polish and the featur
featuree inte
interce
rcepti
ptions
ons of the hor
horizon
izontal
tal scan lin
lines
es with the
number
num ber of field
fieldss to be meas
measure
ured,
d, the fields can be alig
aligned
ned vertically oriented oxides and sulfides and divide this number
contiguously or spaced apart somewhat. Field areas should not by the total length of the horizontal scan lines per field as:
be overlapped. If the fields are aligned contiguously over a N i
square or rectangular area, after examination of the fields, the N L 5 (3)
LT
detec
detected
ted fe
featu
ature
ress in th
thes
esee fie
field
ldss ca
can
n be ad
adde
ded
d to
toge
geth
ther
er to
minimizee edge corre
minimiz correction
ction prob
problems.
lems.
Forr so
Fo soft
ftwa
ware
re-b
-bas
ased
ed sy
syst
stem
ems,
s, wh
wher
eree th
thee pi
pixe
xell ro
rows
ws,, an
12.3.2
12.3.2 For a given inclusion content,
content, the statistical precision
precision artificially
artifici ally created
created grigrid,
d, or som somee othother
er app
approa
roach
ch is useusedd to
of the measurements improves as the area measured increases. produce
prod uce interc
intercept
ept count
counts, s, the longitudinal
longitudinal directi
direction
on must be
The measured area depends on the size of each field, which perpendicular to the intercept count direction. N L is determined
decreases
decreas es with increasing magnification,
magnification, and the numb numberer of in the same manner except that LT must be based on the true
fieldss meas
field measure
ured.
d. The num
number
ber of field
fieldss mea
measur
sured
ed sho
should
uld be length of the pixel rows or the artificial grid lines. For either
based on the relative accuracy of the measurements as defined type of measurement, store in the computer memory N L and N L
in 13.4
in 13.4 or
or by agreement between producer and purchaser. 2
for each type of inclusion (sulfide and oxide) or constituent.
12.3.3
12.3.3 When the sections
sections are sta
stacke
ckedd with
within
in a mou
mountnt to 12.5.5
12.5. 5 If field measurements
measurements are employedemployed to determine the
produce the desired measurement area, stage movement must inclusion or particle lengths (in the hot working direction), for
be carefully adjusted so that the interface between two adjacent each fiel
field d tha
thatt con
contain
tainss inc
inclus
lusion
ionss or par
particl
ticles,
es, meas
measureure the
specimens is not included within the measurement field. total
total pro
project
jected
ed len
length
gth,, H T , (i
(inn µm
µm)) of ea each
ch in
incl
clus
usio
ion
n or
12.4 Setting Up the Computer : preci
precipi
pitat
tatee ty
type
pe.. St
Stor
oree in th thee cocomp
mput
uter
er mem
memor ory
y ththee to
total
tal
12.4.1
12.4.1 The com
comput
puter
er pro
progra
gramm dev
develo
eloped
ped for dat
dataa inp
input,
ut, project
pro jected
ed leng
lengthth per field and the num number
ber of inc
inclus
lusion
ionss per
image analyzer control, measurement, and data analysis is read field, N i, fo
forr ea
eachch ty
type
pe of in inclu
clusision
on (s
(sul
ulfid
fidee an
andd ox
oxid
ide)
e) or
into the central processing unit to commence analysis. Input constituent.
data regarding the specimen identity, data requester, calibration 12.5.6
12.5. 6 If feature-specific
feature-specific measurements
measurements are used to deter deter--
constant,
consta nt, date, number of fields, field spacing, and so forth, are mine th
mine thee sisize
ze of ththee in
inclu
clusio
sions
ns or papart
rtic
icles
les,, me
meas asururee ththee
entered. inclusion length (in the hot working direction) and area for
12.5 Measurement of Stereological Parameters: each inclusion in the field. A protocol must be employed to
12.5.1
12.5. 1 All the stereological
stereological measurements
measurements can be performed
performed correct for edge effects for inclusions or particles lying on a
as field measurements.
measurements. Two measurements,
measurements, the inclus
inclusion
ion or field boundary to ensure that these inclusions or particles are
constituent length and area, also can be performed as feature- properly measured only once. Store in the computer memory
specific measurements, if desired, although this may be slower. the length, Li, and area, A i, of each measured inclusion (sulfide
12.5.2
12. 5.2 For each field, focfocus
us the image (manually
(manually or aut
auto-
o- and oxide) or constituent type.
matically)) and measur
matically measuree the area fraction of the detecte
detected
d oxides 12.5.7
12.5. 7 Move the stage to the next field, refocus, and repeat repeat
and sulfides by dividing the detected area of each by the area the measurements described in 12.5.1-12.5.6
in 12.5.1-12.5.6.. Add the second
of the measurement field or by dividing the total number of set of field measurements ( A A, A A 2, N A, N A 2, N L , N L 2, H T ,
detected picture points by the total number of picture points in N i) to th
thee fir
first
st se
set,
t, an
and
d so fofort
rth,
h, as th
thee nu
numb
mberer of fie fieldldss
-
defined by:
,
,
,
`
`
meas
me asur
urem
emen entt sq
squa
uare
redd fo
forr eac
each h in
incl
clus
usio
ionn ty
type
pe (o (oxi xide
de an andd
`
,
sulfide)
sulfid e) or co cons nstit
titue
uent
nt ty
type
pe foforr n fields.
fields. Altern
Alternatively
atively,, if
`
`
`
`
, Ai PPi
V V 5 A A 5 5 (1) computer memory is not a problem, store each field value of
,
,
,
`
`
,
-
AT PPT
`
-
`
,
,
A A, N A and N L . For the feature-specific measurements L i and
`
separa
sep arated ted,, per
perfor
form m the meas
measureuremen
ments ts des
descri
cribed
bed in 12.5.1-
100. Store in the computer memory the volume fraction and the
12.5.6 on all of the inclusions. For other metals, perform the
12.5.6
volume fraction squared of the sulfides and oxides.
measurements on the constituents present either separately or
12.5.3
12.5.3 For each field, count the numbe
numberr of discre
discrete
te oxides
collectively as required by the application.
and sulfides and divide each number by the field area (mm2) toto
12.5.9
12.5. 9 If exogenous
exogenous inclusions are observed on the plane-
define the number per unit area in accordance with:
of-polish of a test specimen, the approximate length and width
N i of the exo exogen
genousous mat matter
ter sho
should
uld be measmeasure
uredd and rep
report
orteded
N A 5 (2)
AT sepa
separa ratel
telyy. Th
Thee de deptpth
h of ththee ex
exogogen
enou
ouss in
inclu
clusi
sion
on ca
can
n be
determ
det ermine ined,
d, if desdesire
ired,
d, by sect
section
ioning
ing thr
throug
oughh the inc
inclus
lusion
ion
A counting
counting protocol
protocol mus
mustt be cho
chosen
sen to cor
correc
rectt for edge perpendicular to the original sectioning plane. Because exog-
effects so that an inclusion or constituent lying across a field enous inclusions
inclusions are not rando randomly
mly distrib
distributed,
uted, stereological
stereological
boundary is counted only once. Store in the computer memory measurement
measur ement methods
methods are not appropriate.
appropriate. A new specimen for
the number per unit area and the number per unit area squared stereological measurement of the indigenous inclusions should
of the oxides and sulfides. be pre
prepar pared
ed fro
from m an adjaadjacen
centt sect
section
ion,, or aft
after
er a cut
cut-ba
-back,
ck,
E 1245 – 03 (2008)
depending on the nature of the application, or as defined by The value of each measurement is expressed as the mean
other specifications, or as defined by purchaser-producer agree- value plus or minus the 95 % CI. Table
CI. Table 1 lists
1 lists the values of t
t as
as
ments. a function of n
n . Over n = 30, the value of t
t may
may be defaulted to
12.5.10 Ratio parameters, such as the average inclusion area a value of 2.
or the mean free path, based on field measurements should be 13.4 Next, calculate
calculate the percent relative
relative accuracy,
accuracy, % RA, of
calculated (as described in 13.7
in 13.7,, 13.8
13.8 and
and 13.10
13.10)) only from the each measurement for oxides and sulfides by:
¯
mean values of Ā ¯ ¯
A A, N A and N L after all the n fields have been 95 % CI
assessed. Do not determine L ¯ , A
L̄ Ā¯ and l for each field. % RA 5
¯
3 100 (7)
X
13. Calc
Calculati
ulation
on of Resul
Results
ts
13.1 After
13.1 After th thee de
desirsired ed nu
numb
mber er of fie field lds,
s, n, ha have
ve bebeen
en The relative accuracy is an estimate of the percent of error of
each measurement as influenced by the field-to-field variability
measured, calculate the mean value of each field measurement
of the values.
( A A, N A, N L ) stored in memory by dividing the sum of each
13.5 If the percent relative
relative accuracy is too high, more
more fields
measurement for n fields by n to determine the average area
¯ A (as a fraction or as a percentage, as desired), the can be mea
measur
sured.
ed. As the area fra
fractio
ction
n dec
decrea
reases,
ses, it wil
willl be
fraction A Ā
¯ A (per mm2), and the average difficult to obtain percent of RA values below 30 %. For very
average number per unit area N
¯ L (per mm). Alterna- low area (volume) fractions, percent
percent RA values less than 100 %
number of interceptions per unit length N
may be difficult to obtain within a practical measurement time.
tively, if the individual field values of A A A, N A and N L have been
For most work, the number of fields measured should be in the
stored, compute the mean of each in the usual way (the sum of
range of from 200 to 300. A greater number of fields, that is,
the measur
measurements ements divided by n ) for each inclusion (oxide and
¯ (in µm2) and greaterr measur
greate measurement
ement area, may be employed depending
depending on the
sulfide) or constituent type. The average area A Ā
requir
req uiremen
ementsts of the stu
study
dy.. How
Howeve
ever,
r, as the are
areaa meas
measure
uredd
the aveaveragragee len length L̄¯ (in µm
gth L µm)) foforr ox oxid
ideses anand d su sulfi
lfide
dess ar
aree
increases, the improvement in the percent of relative accuracy
calculated by dividing by the number of fields with detectable
decreases and, beyond some number of fields (area measured),
oxid
ox ides
es an and d su sulfi
lfide
dess ra rath ther
er th
than
an th thee to
total
tal nu numbmber er of fiefield
ldss
the improvement in the percent relative accuracy will be small
(un
(unless
less all fiel
fides). fields
ds mea
measursured
ed hav
havee det
detecta
ectable
ble oxi
oxides
des and sul sul-- compared
compar ed to the req
requir
uired
ed ef
effor
fort.
t. For steels with very low
inclusion contents where the percent of relative accuracies of
13.2 If the A A, A A 2, N A, N A 2, N L , and N L 2 have been
the sum of A
the measurements are relatively high, measurement of 200 to
stored in memory, calculate the standard deviation of the field
300 fields per specimen on a larger number of specimens is
measures
measur es by:
recommended rather than measuring 500 or more fields on a
( X 2 2 1/2
s 5
nF 2
( X
n F G G (4)
smaller number of specimens. This procedure produces better
statistical definition of the inclusions in the lot.
13.6
13.6 If the incl
inclusi
usions
ons cannot
cannot be sep
separa
arated
ted by typ
typee and are
If the individual field measurements of A A, N A, and N L have analyz
ana lyzed
ed col
collect
lective
ively
ly,, or if oth
other
er con
constit
stituen
uents
ts are ana analyz
lyzed
ed
been stored in memor
memory y, calculat
calculatee the standard deviation ac- separately or collectively for metals other than steels, apply the
cording to: analytical treatment as described in 13.1-13.5
13.1-13.5 as appropriate.
¯ ! 2 1/2 13.7 If field measurements
measurements of the total projected length of
s 5 F
(~ X i 2 X
n 2 1 G (5) each inclusion or particle type have been made, calculate the
average length of each inclusion or particle type, L L̄¯ , according
to:
con
OTE 2—The dispersion of inclusion field measurement data does not
Nform
confor m to the ide
ideal
al Gau
Gaussi
ssian
an (no
(norma
rmal)
l) for
form
m and the dev deviat
iation
ion fro
from
m ( H T
¯ 5
L
L̄ (8)
normalcy increases as the inclusion content decreases. Thus, the arith- ( N i
metic standard deviation, calculated by (Eq 4 or Eq 5), does not accurately L̄¯ are in µm.
where H T and L
describe the dispersion of the test values about the arithmetic mean of
13.8 If feature-specific
feature-specific measurements
measurements of inclus
inclusion
ion or con-
thesee mea
thes measur
sureme
ements
nts.. The tru
truee dat
dataa dis
disper
persio
sion
n can be defi defined
ned by the
stituent areas have not been made, use the average values of Ā A¯ A
four-moment method5 and calculation of the geometric mean, geometric
-
-
`
,
`
standard
standa rd deviat
deviation,
ion, skew
skew,, and kurtos
kurtosis.
is. Howe
However
ver,, such calcul
calculations
ations are
,
,
`
,
,
,
TABLE 1 95 % Confidence Interval
Interval Multipliers
Multipliers
beyond
bey ond the sco
scope
pe of this pra
`
`
`
,
practic
ctice.
e. Alt
Althou
hough
gh the ariarithm
thmetic
etic sta
standa
ndard
rd
`
deviation does not accurately define the data dispersion for these mea-
`
`
`
,
No. of Fields, n
Fields, n t No. of Fields
Fields,, n t
,
,
NOTE 3—The standard deviation of the mean free path can only be
`
-
`
,
,
6 2.571 19 2.101
`
E 1245 – 03 (2008)
¯ A (determined in 13.1
and N in 13.1)) to calcula
calculate
te the averag Ā¯ , of
averagee area, A 14.7 If the oxides and sulfides cannot cannot be separated and are
each inclusion or particle type by: measured collectively, list the values for all inclusions for each
¯ sample
sam ple and calc
calcula
ulate
te lot ave
averag
rages.
es. If oth
other
er con
constit
stituen
uents
ts are
A
Ā A
¯ 5
A
Ā (9) analyz
ana lyzed
ed sep
separa
arately
tely or col
collect
lective
ively
ly in spe
specime
cimens
ns oth
other
er tha
thann
¯
N
A
steels,
stee ls, list the meas
measure
ured
d ave
averag
rages
es per spespecime
cimen n und
under
er the
where A Ā¯ A must be expressed as a fraction (not as a percent- appropriate
appro priate identifying
identifying headin
headings
gs and calcula
calculatete lot averag
averages.
es.
age). Since N ¯ A is the number per mm2, multiply A Ā¯ by 10 6 to Next, calculate the standard deviation, 95 % CI and percent RA
obtain the mean area in µm 2.
-
-
13.9
13. 9 If fea featurture-s
e-spec
pecific
ific meas
measure
uremen
ments ts of the inc inclus lusion
ion or
,
14.8
14 .8 Fo
Forr th
thee ox
oxid
ides
es an
and
d su
sulfi
lfide
des,
s, or ththee to
total
tal in
inclu
clusio
sion
n
`
,
,
`
,
,
particl
par ticlee len
length gth and are areaa hav
havee bee
been n meas measure
ured,d, Li and A i, `
-
`
-
con
conten
tent
ted,
if list
measur
mea sured
ed
lot col
collect
lective
ively
es ly,
, oreach
for measureme
other
other ement
constit
con stituen
nt uentsts
,
respec
respective
tively ly,, com comput putee the mean
mean,, L Ā indivi
ividua
duall measur
mea sured, the averag
ave rages for measur type,
typ e,
`
,
,
,
,
`
follo
followe
wedd by th thee st
stan
anda
dard
rd de
devi
viati
ation
on,, th
thee 95 % co confi
nfide
denc
ncee `
,
`
`
`
grams of length or area, if desired. The standard deviation of interval, and the percent relative accuracy.
,
,
,
`
,
,
14.9 Repor
Reportt the locatio
locationn and size of any exogeexogenous
nous inclu- `
-
-
where l is th
thee me
mean
an fr
free
ee pa
path
th pe
perp
rpen
endi
dicu
cular
lar to th thee ho hott than 5° from the longitudinal axis must be avoided.
working axis in µm of each inclusion or constituent type, A ¯ A is
Ā 15.2 Voids in the microstructuremicrostructure due to solidification,
solidification, inad-
expressed
expres ¯ L (the mean
sed as a fraction (not as a percentage) and N equate hot ductili ductility ty,, impro
improper
per hot worki
workingng practices, or im-
number of intercepts per mm) must be multiplied by 1000. proper polishing will be detected as oxides and bias the volume
fraction and number per unit area to higher values. The average
14. Test Report
Report area, average length, and mean free path will be biased towards
14.1 The report should document the identif identifying
ying informa- lower values.
tion in 12.4.1
in 12.4.1 regarding
regarding the specimen, its origin, data requester, 15.3
15. 3 The presenc presencee of dust or oth other
er debris
debris on the pol polish
ished
ed
date of analysis, and so forth as needed. surface or dust in the imaging system will bias results towards
14.2 List the number of fields measured,
measured, the area per field higher values.
and the total measurement area. 15.4
15. 4 Imp
Improp roper er sta
stage
ge movmoveme
ementnt con
contro
troll tha
thatt per
permits
mits the
14.3 For the measured quantities
quantities of each inclusion (sulfides
(sulfides objective to measure the mount or free space will bias results.
and oxi
oxides
des)) or con
constit
stituen
uentt par
particl
ticlee typ
type,
e, list eac
each
h mea
measur
sured
ed 15.5
15. 5 Vibribratio ations ns tha
thatt afaffect
fect the dete
detected
cted imag
imagee will bia biass
value, the standard deviation, the 95 % confidence interval, and results.
the percent relative accuracy. For the ratio parameters, list only 15.6 The choice of the magnification magnification used will will influence test
the calculated mean value. This information may be tabulated results.
result s. In general, specimens with large inclus inclusions
ions must be
in several ways depending on the needs of the application. If examined at lower magnifications than specimens with a low
indivi
ind ividua
duall meas
measureuremen
mentsts of leng
length
th and areareaa hav
havee bee
been n ob- density of small inclusions. Inclusions that intersect the frame
tained, these results may be plotted in histogram manner, if border will be partially detected and a relatively low magnifi-
desired. cation reduces this problem. For specimens with very small
14.4 This format
format is repeated for each specimen
specimen in the lot. inclusions,
inclus ions, higher magnifications
magnifications must be emplo employedyed for ad-
14.5 For all of the specimens in the lot, list the mean values equate detection and measurement. However, as the magnifi-
forr in
fo inclu
clusio
sion
n (o (oxi
xide
de anandd su
sulfid
lfide)
e) or cocons
nstit
titue
uent
nt tytype
pe peperr cation increases, the field area decreases and the field-to-field
specimen
specime n and compu
compute te average values of each measurement
measurement to variability, which influences the standard deviation, increases.
produce lot averages. As the magnification is decreased, the N A value will decrease
14.6
14 .6 For
For alalll of th
thee sp
spec
ecim
imen
enss in th
thee lo
lot,
t, co
comp
mpututee th
thee and
an d th L̄¯ , A
thee L ¯ and l
Ā l̄¯ va
valu
lues
es in
incr
creas
easee be
becacaus
usee th
thee sm
small
aller
er
standard deviation (in accordance with (Eq 4 or Eq 5)), the inclusions will not be detected. Consequently, results should
95 % CI (in accordance with (Eq 6)) and the percent RA (in not be compa
compared red if signifi
significantly
cantly different
different objective magnifica-
accordance with (Eq 7)) for each measurement type to assess tions were used for measurements. The same objective should
the statistical value of the data. For these calculations, n is the be used for all measurements of specimens in the same lot.
numberr of specim
numbe specimens
ens in the lot rather than the numb
number er of fields Low magnification objectives should be avoided. Intermediate
measured. magnification objectives, e.g., 323 40 3, 503, 603 and 803,
NOTE 4—The comments in Note 2 (after 13.2)
13.2) do not apply in this provide the best combination of resolution and field size. As
situation because the dispersion of the mean values for each specimen the A A value
value dec decrea
reasesses,, the ave
averag
ragee inc
inclus
lusion
ion size usuusually
ally
about their mean (heat average) will be Gaussian (normal). decreases, and higher magnification objectives are required.
E 1245 – 03 (2008)
15.7 Impro
Improper
per setting of the threshold ranges for detection
detection 15.10 Cha
15.10 Charact
racteri
erizati
zation
on of the inc
inclus
lusion
ion con
conten
tentt with
withinin a
and discrimination of phases or inclusions will bias results. If given heat lot, or a subunit of the heat lot, improves as the
the detection scheme appears to be inadequate, the operator number of specimens measured increases. For the testing of
should abort the run and reset the threshold levels. billets rolled from ingots, the practice of sampling only the
15.8 The precision
precision of the measurements
measurements is a direct function
function extreme tops and bottoms may not be representative of the bulk
of the measurement area, that is, the field size and the number material. These locations may present extremes in the oxide
of fields measured. Hence, precision can be improved simply and sulfide contents. The addition of billet locations
locations within the
by inc
increas
reasing
ing the num
number
ber of mea
measur
suremen
ementt field
fieldss unt
until
il the ingot is recommended to include conditions representative of
percent of relative accuracy reaches the desired level. As the thee bu
th bulk
lk of th
thee ma
mater
teria
ial.
l. Lik
Likew
ewis
ise,
e, fo
forr a he
heat
at of ststeel
eel,, th
thee
volume
ment areafraction of the inclusions
is required to obtain andecreases, a greater
acceptable measure-
precision. For inc
inclus
lusion
ion Hence,
sequence. conten
con tentt asmay vary
vary sub
the number substa
ofstantia
ntially
lly wit
within
systematically hin the ing
selectedingot
ot
test
very
ver y low incinclus
lusion
ion con
conten
tentt spe
specime
cimens,
ns, thi
thiss may req
requir
uiree a locatio
locations
ns inc
increa
reases
ses,, the abi
ability
lity to cha
charac
racter
terize
ize the incl
inclusi
usion
on
prohib
pro hibitiv
itivee amo
amount
unt of mea
measursureme
ement
nt time
time.. A poi
point
nt wil
willl be cont
conten
entt im
impr
prov
oves
es.. ThThee sam
samee ru
rule
less ap
appl
ply
y to sam
samplplin
ing
g of
reached
reac hed where the add additio
ition
n of mor
moree fiel
fields
ds yie
yields
lds very litt
little
le continuous
contin uously
ly cast materia
material.
l.
improvement in the percent relative accuracy. At this point, it
is impractical to continue the analysis. Field areas should be 16. Keyw
Keywords
ords
spaced apart or aligned contiguously, never overlapped. 16.1 exoge
exogenous
nous inclus
inclusion;
ion; featur
feature-spe
e-specific
cific measur
measurements;
ements;
15.9
15.9 If the spespecime
cimenn is rep
repoli
olishe
shed
d so that a new parallel
parallel field measur
measurements;
ements; image analys
analysis;
is; inclus
inclusions;
ions; indig
indigenous
enous
plane is measured, reproducibility will not be as good as when inclusions;
inclus ions; light micros
microscopy
copy;; oxide
oxide;; secon
second-pha
d-phase
se particl
particles;
es;
the same plane is remeasured. statistical
statistical analys
analysis;
is; stereo
stereology;
logy; sulfid
sulfidee
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validity
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ned
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-
-
-
`
,
,
`
,
`
,
,
`
,
,
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