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: D4541 − 17
Standard Test Method for
Pull-Off Strength of Coatings Using Portable Adhesion
Testers1
This standard is issued under the fixed designation D4541; the number immediately following the designation indicates the year of
original
origin
al adoption or, in the case of revis
revision,
ion, the year of last revision.
revision. A number in paren
parenthese
thesess indicates the year of last reappr
reapproval.
oval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Sco
Scope*
pe*
that co
that
coati
ating
ngss ca
can
n be tes
teste
ted
d ev
even
en th
thou
ough
gh on
only
ly on
onee si
side
de is
accessible. Measurements are limited by the strength of adhesive
si
ve bo
bond
ndss be
betw
twee
een
n th
thee lo
load
adin
ing
g fix
fixtu
ture
re an
and
d th
thee sp
speci
ecime
men
n
surface or the cohesive strengths of the glue, coating layers,
and substrate.
1.1 This test method covers a procedure for evaluating
evaluating the
pull-offf str
pull-o
streng
ength
th (co
(commo
mmonly
nly ref
referr
erred
ed to as adh
adhesio
esion)
n) of a
coating
coa
ting sys
system
tem fro
from
m meta
metall sub
substr
strates
ates.. Pul
Pull-o
l-offf str
streng
ength
th of
coatingss from concrete
coating
concrete is described in Test Method D7234.
D7234.
This test offers two test protocols. Protocol 1 (test to fracture)
determines the greatest perpendicular force (in tension) that a
surface area can bear before a plug of material is detached.
Protocol 2 (pass/fail) determines if the coated surface remains
intact at a defined load criteria. Fracture will occur along the
weakest plane within the system comprised of the test fixture,
glue, coating system,
system, and substr
substrate,
ate, and will be exposed by the
fracture surface. This test method maximizes tensile stress as
compared
compar
ed to the shear stress applied by other methods,
methods, such as
scratch or knife adhesion, and results may not be comparable.
1.4 Thi
Thiss test can be destructiv
destructivee and spot repairs
repairs may be
necessary.
1.5 The values stated in either SI units or inch-pound
inch-pound units
are to be regarded separately as standard. The values stated in
each system may not be exa
exact
ct equ
equival
ivalent
ents;
s; ther
therefo
efore,
re, eac
each
h
system shall be used independently of the other. Combining
values from the two systems may result in non-conformance
with the standard.
standard
d doe
doess not purport
purport to add
addre
ress
ss all of the
1.6 This standar
safe
sa
fety
ty co
conc
ncern
erns,
s, if an
anyy, as
asso
socia
ciated
ted wi
with
th its us
use.
e. It is th
thee
responsibility of the user of this standard to establish appro priate safety, health and environmental practices and determine the applicability of regulatory limitations prior to use.
1.7 This inte
interna
rnatio
tional
nal sta
standa
ndard
rd was dev
develo
eloped
ped in acc
accor
or-dance with internationally recognized principles on standardizat
iz
atio
ion
n est
estab
ablis
lishe
hed
d in th
thee De
Deci
cisio
sion
n on Pr
Prin
incip
ciples
les fo
forr th
thee
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical
Barriers to Trad
Tradee (TBT) Committee.
NOTE 1—The
1—The pro
proced
cedure
ure in thi
thiss sta
standa
ndard
rd was dev
develo
eloped
ped for met
metal
al
substrates, but may be appropriate for other rigid substrates such as plastic
and wood. Factors such as loading rate and flexibility of the substrate must
be addressed by the user/specifier.
NOTE 2—The procedure in this standard was developed for use on flat
surfaces. Depending on the radius of the surface, the results could have
greater variability with lower values and averages.
1.2 Pull-o
Pull-offf streng
strength
th measu
measurements
rements depend upon material
material,,
instrumentation and test parameters. Results obtained by each
test method may give different results. Results should only be
assessed for each test method and not be compared with other
instruments.
instru
ments. There are five instrument types, identified as Test
Methods B-F. It is imperative to identify the test method used
when repor
reporting
ting results
results..
2. Referenc
Referenced
ed Documents
2.1 ASTM Standards: 3
D2651 Guide
D2651
Guide for Preparation
Preparation of Metal Surfaces for Adhesive
Bonding
D3933 Gui
Guide
de for Pre
Prepar
paratio
ation
n of Alu
Alumin
minum
um Sur
Surfac
faces
es for
Structural
Structu
ral Adhes
Adhesives
ives Bondi
Bonding
ng (Phos
(Phosphor
phoric
ic Acid Anodizing)
D7234 Test
D7234
Test Method for Pull-Off Adhesion Strength of Coatings on Concrete Using Portable Pull-Off Adhesion Testers
E691 Practic
Practicee for Condu
Conducting
cting an Interl
Interlabora
aboratory
tory Study to
Determine the Precision of a Test Method
NOTE 3—Meth
3—Method
od A, whi
which
ch app
appear
eared
ed in pre
previo
vious
us ver
versio
sions
ns of thi
thiss
standard, has been eliminated as its main use is for testing on concrete
substrates (see Test Method D7234
Method D7234).
).
1.3 This test method describes
describes a class of apparatus known as
portable pull-off adhesion testers.2 They are capable of applying a concentric load and counter load to a single surface so
1
This test method is under the jurisdiction of ASTM Committee D01
Committee D01 on Paint
and Related Coatings, Materials, and Applications and is the direct responsibility of
Subcommittee D01.46
Subcommittee
D01.46 on Industrial Protective Coatings.
Current
Curre
nt editio
edition
n approv
approved
ed Aug. 1, 2017. Published
Published Sept
September
ember 2017. Origin
Originally
ally
approved in 1993. Last previous edition approved in 2009 as D4541 – 09 1. DOI:
10.1520/D4541-17.
2
The term adhesion tester may be somewhat of a misnomer, but its adoption by
two manufacturers
manufacturers and at least two patent
patentss indica
indicates
tes continued usage.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
ɛ
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
D4541 − 17
3. Summ
Summary
ary of Test
Test Method
5. Appar
Apparatus
atus
3.1 The gen
genera
erall pul
pull-o
l-offf test is per
perfor
formed
med by sec
securi
uring
ng a
loading
load
ing fixt
fixture
ure (do
(dolly
lly,, stu
stud)
d) nor
normal
mal (pe
(perpe
rpendi
ndicul
cular)
ar) to the
surface of the coating with a glue. After the glue is cured, a
testing apparatus is attached to the loading fixture and aligned
to apply tension normal to the test surface. The force applied to
the loading fixture is then gradually and uniformly increased
and monitored until either the loading fixture is detached, or a
specified load value is reached and the test terminated. The two
common uses of this test are test to fracture (Protocol 1), and
pass
pa
ss/f
/fail
ail tes
testin
ting
g (P
(Pro
roto
toco
coll 2)
2).. Tes
estt to fr
frac
actu
ture
re is us
used
ed to
determine a maximum load that can be achieved when a plug
of material is detached with the selected testing parameters.
Pass/fail is used to verify the results of a testing procedure can
meet a minimum load criterion. When the loading fixture is
detached, the exposed surface represents the plane of limiting
strength within the system. The nature of the plane of fracture
is qua
qualifi
lified
ed in acco
accorda
rdance
nce wit
with
h the per
percen
centt of adh
adhesiv
esivee and
cohesive failures, and the actual interfaces and layers involved.
The reported load is computed based on the maximum indicated
cate
d loa
load,
d, the ins
instru
trumen
mentt cali
calibra
bratio
tion
n dat
data,
a, and the ori
origin
ginal
al
surfac
sur
facee are
areaa str
stress
essed.
ed. Resu
Results
lts obt
obtain
ained
ed usi
using
ng dif
differ
ferent
ent test
devices will vary because the results depend on instrumentation parameters. Variations in results are also expected when
tests are performed under different test procedures or environmental conditions (see 4.2
4.2)).
5.1 Adhesion Tester, commercially available, or comparable
apparatus
appar
atus to the specific examples listed in Annex
in Annex A1 – Annex
A5..
A5
5.1.1 Loading Fixtures, having a flat surface on one end that
can be adhered to the coating and a means of attachment to the
tester on the other end. Optimal size of the loading fixture is
determined by the adhesion tester capabilities. The fixture and
tester
test
er com
combin
binatio
ation
n sho
should
uld be cho
chosen
sen so tha
thatt the exp
expecte
ected
d
maximum pull load the coating will be subjected to during the
test is within the range of the tester.
5.1.2 Detaching Assembly (adhesion tester), having a central grip for engaging the fixture.
5.1.3 Base, on the detaching assembly, or an annular bearing
ring
rin
g if nee
needed
ded for uni
unifor
formly
mly pre
pressin
ssing
g aga
agains
instt the coa
coatin
ting
g
surfac
sur
facee aro
around
und the fixt
fixture
ure either directly
directly,, or by way of an
interm
int
ermedi
ediate
ate bea
bearin
ring
g rin
ring.
g. A mea
means
ns of alig
alignin
ning
g the bas
basee is
needed so that the resultant force is normal to the surface.
5.1.4 Means of moving
moving the grip away from
from the base to allow
the loading of the fixture in as smooth and uniform a manner
as possible and so that a torsion free, co-axial (opposing pull of
the grip and push of the base along the same axis) force results
between
betwee
n them.
5.1.5 Timer, or means
means of limiting
limiting the loading
loading rate. A timer is
the minimum equipment when used by the operator along with
the force indicator in 5.1.6
5.1.6..
5.1.6 Forc
Forcee Ind
Indica
icator
tor and Cal
Calibr
ibrati
ation
on Inf
Inform
ormatio
ation,
n, for
determining the actual force delivered to the loading fixture.
4. Sign
Significan
ificance
ce and Use
5.2 Solvent, or other means for cleaning the loading fixture
surface.
surfa
ce. Finger prints, moisture, oxides, and dust tend to be the
primary contaminants.
4.1 Th
4.1
Thee pu
pullll-of
offf st
stre
reng
ngth
th of a co
coati
ating
ng is a pe
perf
rfor
orma
manc
ncee
proper
pro
perty
ty that may be ref
refere
erence
nced
d in spe
specific
cificatio
ations.
ns. Thi
Thiss test
method serves as a means for uniformly preparing and testing
coated surfaces, and evaluating and reporting the results. This
test method is applicable to any portable apparatus meeting the
requirements for determining the pull-off strength of a coating
in this standard (see Annexes).
5.3 Sandpaper, or other means, used to roughen the surfaces
for glue application and adherence to the coating. When using
sandpaper it is recommended to use 100 grit or finer.
5.4 Glue— the
the material used for securing the loading fixture
to the coating. Two component epoxies and cyanoacrylates are
two commonly used glues. Select a glue that does not affect the
coatin
coa
ting
g pro
proper
perties
ties,, flow thr
throug
ough
h the coa
coatin
ting
g or atta
attack
ck the
coating.
4.2 Vari
ariatio
ations
ns in res
result
ultss with the same coating
coating are lik
likely
ely
when an
when
any
y pa
para
rame
meter
ter of th
thee tes
testt is ch
chan
ange
ged.
d. Th
This
is in
inclu
clude
dess
change in glue, load fixture size, substrate coating cure time,
pull rate, environmental conditions, if the coating is scored, or
using a different device. Therefore, when a series of results will
be compared with one another or used for statistical analysis,
the type of apparatus, substrate, test procedures, glue type, and
if scoring is used should be the same for the pulls considered. 4
It is recommended that these parameters and the environmental
conditions allowed during the test be mutually agreed upon
between the interested parties.
5.5 Clamps, magnetic, mechanical, tape or similar, if needed
for holding the fixture in place while the glue cures.
5.6 Cotton Swabs, or other means for removing excess glue
and defi
definin
ning
g the adh
adhere
ered
d are
area.
a. Any meth
method
od for removing
removing
excess glue that damages the surface, such as scoring (see 6.7
6.7),
),
mustt gen
mus
genera
erally
lly be avo
avoide
ided
d sin
since
ce ind
induce
uced
d sur
surfac
facee flaw
flawss may
cause premature failure of the coating.
5.7 Scoring Tool, circular hole cutter, or similar tool to score
through to the substrate around the loading fixture.
4.3 The purchaser
purchaser or specifier shall
shall designate a specific test
method procedure; B, C, D, E, or F and test Protocol; 1, or 2,
when
wh
en ca
calli
lling
ng ou
outt th
this
is st
stan
anda
dard
rd.. In cas
cases
es wh
wher
eree eit
eithe
herr th
thee
Protocol or a pass/fail criterion is not designated, Protocol 1
shall be used.
6. Test Preparation
Preparation
6.1 The method for selecting
selecting the coating
coating sites to be prepared
forr te
fo
test
stin
ing
g de
depe
pend
ndss up
upon
on th
thee ob
obje
ject
ctiv
ives
es of th
thee te
test
st an
and
d
agree
ag
reemen
ments
ts be
betwe
tween
en the co
contr
ntract
acting
ing par
partie
ties.
s. Th
Ther
eree ar
are,
e,
however, a few physical restrictions imposed by the general
method and apparatus. The following requirements apply to all
sites:
4
Reference to potential variability of the adhesion test has been made in various
publications, including the assessment of variability completed for the test method
found in ASTM Research Report RR:D01-1147.
2
D4541 − 17
6.1.1 The selected test area must
must be large enough to accomaccommodate the specified number of replicate tests. The surface may
have any orientation with reference to gravitational pull. Each
load
lo
adin
ing
g fix
fixtu
ture
re mu
must
st be se
sepa
para
rate
ted
d by at le
least
ast th
thee di
dist
stan
ance
ce
needed to accomm
accommodate
odate the detach
detaching
ing apparatus. For Proto
Protocol
col
1 or to sta
statis
tistic
ticall
ally
y ch
char
aract
acter
erize
ize a te
test
st ar
area
ea,, th
thre
reee or mo
more
re
replications are required.
6.1.2 The selected test areas must also have enough
enough perpendicular and radial clearance to accommodate the apparatus, be
flat enough to permit alignment, and be rigid enough to support
the counter force. It should be noted that measurements close
to an edge may not be representative of the coating as a whole.
preventt micr
preven
micro-c
o-crac
rackin
king
g in the coa
coating
ting or glu
glue,
e, sin
since
ce suc
such
h
cracks may cause reduced values. Scored samples constitute a
different test procedure, and should be clearly reported with the
resu
re
sults
lts.. Sc
Scor
orin
ing
g may be re
requ
quir
ired
ed fo
forr th
thic
ickk-film
film co
coati
ating
ngs,
s,
reinfor
rein
forced
ced coat
coatings
ings and elas
elastome
tomeric
ric coa
coating
tings.
s. Sco
Scoring
ring,, if
performed, can be completed before or after the load fixture is
glued to the coating. When performed, scoring shall be done in
a manner that ensures the cut is made normal to the coating
surface, in a manner that does not twist or torque the test area
or impart the loading fixture, and minimizes heat generation,
edge damage, or microcracks to the coating or glue and the
substr
sub
strate.
ate. For thi
thick
ck coa
coatin
tings
gs it is rec
recomm
ommend
ended
ed to coo
cooll the
coatin
coa
ting
g and sub
substr
strate
ate dur
during
ing the cut
cuttin
ting
g pro
proces
cesss with wat
water
er
lubrication.
6.2 Since the rigidity of the substrate
substrate affects
affects results of the
test an
test
and
d is not a co
con
ntr
tro
oll
llab
able
le te
test
st var
aria
iab
ble in fie
field
ld
measurements, some knowledge of the substrate thickness and
compos
com
positio
ition
n sho
should
uld be rep
report
orted
ed for sub
subseq
sequen
uentt ana
analys
lysis
is or
laboratory
labora
tory comparisons.
comparisons. For examp
example,
le, steel substrate of less
than 3.2 mm (1 ⁄ 8 in.) thic
thickne
kness
ss usu
usually
ally red
reduce
ucess test res
result
ultss
1
compared to 6.4 mm ( ⁄ 4-in.) thick steel substrates.
NOTE 5—A template made from wood with a hole of the same size as
the scoring tool drilled through it and secured to the surface may be an
effective method to limit sideways movement of the scoring tool.
NOTE 6—-Scoring requirements will vary depending on coating system,
chemistry, and thickness. A direct comparison of the unscored result to a
scored result is one method to determine if scoring should be performed.
Other
Oth
er met
method
hodss for mak
making
ing thi
thiss det
determ
ermina
inatio
tion
n may be emp
employ
loyed
ed wit
with
h
agreem
agr
eement
ent bet
betwee
ween
n the pur
purcha
chaser
ser and sel
seller
ler.. Sco
Scorin
ring
g sho
should
uld not be
considered for coatings less than 20 mils.
6.3 Subje
Subject
ct to the requirements
requirements of 6.1,
6.1 , select representative
test areas and clean the surfaces in a manner that will not affect
integrity of the coating or leave a residue. To reduce the risk of
glue fracture affecting the test, the surface of the coating can be
lightly abraded to promote adhesion of the glue to the surface.
If th
thee su
surf
rfac
acee is ab
abra
rade
ded,
d, ca
care
re mu
must
st be tak
taken
en to pr
prev
even
entt
significant loss of coating thickness. Clean the area to remove
particulates after abrading. Use of a solvent may be necessary
to remove all contaminants. If a solvent is required, select one
that does not compromise the integrity of the coating.
6.8 Note the appro
approximate
ximate temperature,
temperature, relativ
relativee humid
humidity
ity,,
and other pertinent environmental conditions during the time of
test.
7. Test Procedure
Procedure
7.1 Test Methods:
Methods:
7.1.1 Test Method A (discontinued).
Test Metho
Method
d B — Fixed Alignment
Alignment Adhes
Adhesion
ion Tester
Tester
7.1.2 Test
Type II:
7.1.2.1
7.1.2
.1 Opera
Operate
te the instru
instrument
ment in accordance with
Annex A1.
A1.
7.1.3 Test Method C — Self-Alignment Adhesion Tester
Type III:
7.1.3.1
7.1.3
.1 Opera
Operate
te the instru
instrument
ment in accordance with
Annex A2.
A2.
7.1.4 Test Method D — Self-Alignment Adhesion Tester
Type IV:
7.1.4.1
7.1.4
.1 Opera
Operate
te the instru
instrument
ment in accordance with
Annex A3.
A3.
7.1.5 Test Method E — Self-Alignment Adhesion Tester
Type V:
7.1.5.1
7.1.5
.1 Opera
Operate
te the instru
instrument
ment in accordance with
Annex A4.
A4.
7.1.6 Test Method F — Self-Alignment Adhesion Tester
Type VI:
7.1.6.1
7.1.6
.1 Opera
Operate
te the instru
instrument
ment in accordance with
Annex A5.
A5.
6.4 Clea
Clean
n the loading
loading fixt
fixture
ure surface
surface as ind
indicat
icated
ed by the
apparatus manufacturer. Failures at the fixture-glue interface
can of
ofte
ten
n be av
avoi
oide
ded
d by tr
treat
eatin
ing
g th
thee fix
fixtu
ture
re su
surf
rfac
aces
es in
accordance with an appropriate ASTM standard practice for
preparing metal surfaces for glue bonding.
NOTE 4—Guides
4—Guides D2651
D2651 and
and D3933
D3933 are
are typical of well-proven methods
for improving adhesive bond strengths to metal surfaces.
6.5 Prepa
Prepare
re the glue in accord
accordance
ance with the glue manufacturer’s recommendations. Apply the glue to the fixture or the
surface to be tested, or both, using a method and thickness
recommended by the glue manufacturer. Be certain to apply the
glue across the entire fixture surface. Position the fixture on the
surface to be tested. Carefully remove any excess glue from
around the fixture. (Warning
( Warning—Movement,
—Movement, especially twisting,
can cau
cause
se tin
tiny
y bub
bubble
bless to coa
coalesc
lescee into large
large hol
holida
idays
ys tha
thatt
constitute stress discontinuities during testing which may lead
to glue fracture.)
6.6 Based on the glue manufacturer’s recommendations and
the anticipated environmental conditions, allow enough time
for the glue to cure. During the glue set and early cure stage,
a constant contact pressure should be maintained on the fixture.
Magnet
Mag
netic
ic or mech
mechanic
anical
al clam
clampin
ping
g sys
system
temss wor
work
k well
well,, but
systems relying on tack, such as masking tape, should be used
with care to ensure that they do not relax with time and allow
air to intrude between the fixture and the test area.
7.2 Select an adhesion-tester
adhesion-tester with a detaching assembly
assembly and
loading fixture size that has a force calibration spanning the
range
ran
ge of exp
expect
ected
ed val
values
ues.. Mid
Mid-ra
-range
nge mea
measur
sureme
ements
nts are
recommended, but read the manufacturer’s operating instructions before proceeding. The adhesion tester shall be calibrated
at the lesser of the manufacturer’s recommended frequency or
every three years.
6.7 Whe
When
n sco
scorin
ring
g aro
around
und the test surface
surface is agr
agreed
eed upon
between the purchaser and seller, extreme care is required to
3
D4541 − 17
7.3 If a bea
bearin
ring
g ring or com
compar
parable
able device
device (5.1.3
( 5.1.3)) is to be
used, place it concentrically around the loading fixture on the
coating surface. If shims are required when a bearing ring is
employed,
employ
ed, place them betwee
between
n the tester base and bearin
bearing
g ring
rather than on the coating surface.
7.4
7.
4 Ca
Care
refu
fully
lly co
conn
nnec
ectt th
thee ce
cent
ntra
rall gr
grip
ip of th
thee de
detac
tachi
hing
ng
assembly to the loading fixture without bumping, bending, or
otherwise prestressing the sample and connect the detaching
assembly to its control mechanism, if necessary. For nonhorizontal
zon
tal sur
surfac
faces,
es, it may be nec
necess
essary
ary with som
somee dev
devices
ices to
suppor
sup
portt the detaching
detaching assembly
assembly so tha
thatt its wei
weight
ght does not
impact the loading fixture and contribute to the force exerted in
the test. Follow the manufacturer’s recommendations.
FIG. 1 Specimen Description
equivalent diameter
diameter of the
the original
original surface
surface area stressed
stressed
d = equivalent
having
hav
ing uni
units
ts of mill
millime
imeters
ters (in
(inche
ches).
s). Thi
Thiss is usu
usually
ally
equal to the diameter of the loading fixture.
7.5 Ali
Align
gn the dev
device
ice acc
accord
ording
ing to the man
manufa
ufactu
cturer’
rer’ss instructions and set the force indicator to zero.
8.3 For tests where the load fixture becomes
becomes detached from
the test
tested
ed sur
surfac
face,
e, vis
visuall
ually
y esti
estimate
mate the per
percen
centt of coa
coatin
ting
g
adhesive and cohesive fracture and glue failure in accordance
to their respective areas and location within the test system
comprised of coating and glue layers. Glue fracture or failure
is defined as a visible separation of the glue from itself, the
coating or load fixture. A convenient scheme that describes the
total test system is outlined in 8.3.1
in 8.3.1 through
through 8.3.3
8.3.3..
8.3.1
8.3
.1 Des
Descri
cribe
be the spe
specime
cimen
n as sub
substr
strate
ate A, upo
upon
n whi
which
ch
successive
succes
sive coatin
coating
g layers B, C , D, etc., have been applied,
including the glue, Y , that secures the fixture, Z , to the top coat
(Fig. 1).
1).
8.3.2
8.3
.2 Designat
Designatee coh
cohesi
esive
ve fra
fractu
ctures
res by the lay
layers
ers wit
within
hin
which they occur as B , C , D , Y , etc., and the visually estimated
percent of each.
8.3.3 Design
Designate
ate adhesive fractures
fractures and glue failure by the
interfaces at which they occur as A/B , B/C , C/D , Y/Z , etc., and
the visually estimated percent of each.
NOTE 7—Pr
7—Prope
operr ali
alignm
gnment
ent is crit
critica
ical.
l. If alig
alignm
nment
ent of the dev
device
ice is
required, use the procedure recommended
required,
recommended by the manufacturer
manufacturer of the
adhesion tester and report the procedure used.
7.6 Incre
Increase
ase the load to the fixture in as smooth
smooth,, consistent,
consistent,
and uniform a manner and rate as possible. The rate of pull
shall be 1 MPa/s (150 psi/s) or less. The rate should be set so
that the test is completed in less than 100 seconds. If multiple
tests are required, the rate of pull shall be similar for each test.
NOTE 8—A change in load fixture
fixture size may result in a change in the rate
of pull depending on the equipment used. A change in rate of pull or load
fixture size will result in variation of results.
7.7 The test is completed when the fixture
fixture is detached from
the sub
substr
strate,
ate, pass/fail
pass/fail test criteria
criteria is met or max
maximu
imum
m pul
pulll
strength for the instrument is reached. For pass/fail tests, the
test may be terminated at any point after the test criterion has
been reached.
8.4 A result that appears to be significantly
significantly different
different from
other results (see repeatability limits in 10.1.1
in 10.1.1)) may be caused
by a mist
mistake
ake in test pro
proced
cedure
ure per
perfor
forman
mance,
ce, rec
record
ording
ing or
calculating. If any of these are not the cause, then examine the
experimental
exper
imental circumstances
circumstances surro
surroundin
unding
g this run. If an irregu
irregu-lar result can be attributed to an experimental cause, drop this
result
res
ult fro
from
m the analysis.
analysis. How
Howeve
everr, do not discard
discard a res
result
ult
unless
unl
ess ther
theree are val
valid
id non
nonstat
statisti
istical
cal rea
reason
sonss for doing so or
unless
unl
ess the res
result
ult is a stat
statisti
istical
cal out
outlier
lier.. Valid non
nonstat
statisti
istical
cal
reasons for dropping results include alignment of the apparatus
that is not normal to the surface, poor definition of the area
stressed due to improper application of the glue, poorly defined
glue lines and boundaries, holidays in the glue caused by voids
or inclusions, improperly prepared surfaces, improperly scored
surfaces, varying the rate of loading during the test, varying the
rate of loading between tests, and sliding or twisting the fixture
duri
du
ring
ng th
thee in
initi
itial
al cu
cure
re.. Sc
Scra
ratc
tche
hed
d or sc
scor
ored
ed sa
samp
mple
less ma
may
y
contain stress concentrations leading to premature fractures.
7.8 Record informatio
information
n required for the Report (see Section
9).
7.9 If a plu
plug
g of material
material is det
detach
ached,
ed, label and store the
fixture for qualification of the failed surface in accordance with
8.3..
8.3
7.10 Rep
7.10
Report
ort any dep
departu
artures
res fro
from
m the pro
proced
cedure
ure such as
possible misalignment, hesitations in the force application, etc.
8. Calc
Calculat
ulation
ion or Inter
Interpre
pretati
tation
on of Resul
Results
ts
8.1 If ins
instru
tructed
cted by the ins
instru
trumen
mentt man
manufa
ufactu
cturer
rer,, use the
instrument calibration factors to convert the indicated load for
each test into the actual load applied.
8.2 Eith
Either
er use the cali
calibra
bration
tion chart
chart sup
supplie
plied
d by the manufacturer or compute the relative load applied to each coating
sample as follows:
X 5 4 F / π d 2
(1 )
8.5 Doc
Docume
ument
nt any tes
testt whe
where
re the loa
load
d limi
limitt of the test
testing
ing
equipment is reached.
where:
greates
atestt mea
mean
n pul
pull-o
l-offf load applied
applied during
during a pas
pass/f
s/fail
ail
X = gre
test, or the pull-off load achieved at fracture. Both have
units of MPa (psi),
F = act
actual
ual load
load applied
applied to the test surfac
surfacee as det
determ
ermine
ined
d in
8.1,, and
8.1
8.6 Proto
Protocol
col 1 (Test to fracture)
fracture) see Fig. 2 Flow
2 Flow Chart.
8.6.1 Unless otherwise
otherwise agreed to between the purchaser
purchaser and
selle
se
llerr, di
disr
sreg
egar
ard
d tes
testt re
resu
sults
lts wi
with
th vi
visu
sual
ally
ly es
estim
timate
ated
d gl
glue
ue
fracture greater than 1/4 of the loading area. Use caution when
using data from tests that include any visible glue fracture or
4
D4541 − 17
FIG. 2 Flow Chart
where the equipment capacity is exceeded for analysis as the
results may not be statistically relevant.
the te
the
test
st pr
proc
oced
edur
uree an
and
d ma
make
ke ad
adju
justm
stmen
ents
ts to re
redu
duce
ce gl
glue
ue
fracture or indicate the test is indeterminate.
NOTE 9—Any amount of glue fracture will result in a reduction of the
maximum test load measured by the testing apparatus
NOTE 10—When subjected to pull-off loads, an elastomeric coating may
elongate, and if the elongation or strain is sufficient, then the failure can
be induced by a simulated peel type load starting at the edges of the scored
sample. To reduce this effect proper scoring and test fixture alignment
techniques
techni
ques should be emplo
employed.
yed. As well, low loading rates shoul
should
d be
avoided to reduce the time the elastomeric coating is under stress. These
factors do not preclude pull-off strength testing of elastomeric materials
but should be noted when evaluating results.
8.7 Proto
Protocol
col 2 (Pass/fail
(Pass/fail test), see Fig.
see Fig. 2 Flow
2 Flow Chart.
8.7.1 The test can be terminated after the minimum
minimum criterion
has been met.
8.7.2
8.7
.2 A test is pas
passin
sing
g whe
when
n the maximum
maximum load applied
applied is
greater than or equal to the pass/fail criteria.
8.7.3 If the maximum load is less than the pass/fail criteria,
criteria,
the test is either a failing test or an indeterminate test due to
glue fracture. A test result is indeterminate when there is a
visible amount of glue fracture (visibly detectable glue fracture
is defined as glue failure of 5 % or more of the loading area)
that occurred during the test and the maximum load is less than
the pass/fail criteria. An indeterminate test may be redone to
determine a passing or failing result. If the test is redone, and
glue fracture persists at a load below the test criteria, review
9. Repor
Reportt
9.1 Report the following
following information:
information:
9.1.1 Date, test location, testing
testing agent,
9.1.2 Brief description
description of the general
general nature of the test, such
as, field or laboratory testing, generic type of coating, etc.
5
D4541 − 17
TABLE 1 Adhesion Testing Method B, Pull-Off Strength ( psi )
9.1.3 Tempe
9.1.3
Temperat
rature
ure and rel
relativ
ativee hum
humidi
idity
ty and any oth
other
er
pertinent environmental conditions during the test period.
9.1.4 Descrip
Description
tion of the apparatus used, including:
including: apparatus man
manufa
ufactu
cturer
rer and mod
model
el num
number
ber,, las
lastt cali
calibra
bratio
tion
n dat
date,
e,
loading
loadin
g fixture type and dimensions,
dimensions, and bearin
bearing
g ring type and
dimensions.
9.1.
9.
1.5
5 De
Descr
scrip
iptio
tion
n of th
thee te
test
st sy
syste
stem,
m, if po
poss
ssib
ible,
le, by th
thee
indexing scheme outlined in 8.3
in 8.3 including:
including: product identity and
generic type for each coat and any other information supplied,
and the substrate identity (thickness, type, orientation, etc.).
9.1.6 Glue used and cure time before
before test.
9.1.7 Method used
used to secure the loading fixture during
during glue
cure, if any.
9.1.8
9.1
.8 Rate of pull.
pull.
9.1.9 Test results.
9.1.9.
9.1
.9.1
1 Deta
Detailed
iled test res
results
ults as des
descri
cribed
bed in
in Fig. 2,
2, Flow
Chart.
Repeatability Reproducibility
Standard
Standard
Deviation
Deviation
x¯
sr
sR
B
1195
27 8
3 30
C
5 49
10 9
117
D
1 21 2
12
41 2
4 83
E
1 38 5
19 2
2 76
Repeatability
Coating
Coatin
g Avera
Average
ge
Limit
x¯
r
% of average
B
1195
77 7
6 9. 1
C
5 49
30 5
5 5. 6
D
1 21 2
1155
9 5 .3
E
1 38 5
53 7
3 8. 8
Avg.
6 4 .7
Coating
Coatin
g Avera
Average
ge
Repeatability
Limit
Reproducibility
Limit
r
R
7 77
92 5
305
32 6
1155
1 3 51
5 37
77 4
Reproducibility
Limit
R
% of average
9 25
7 7 .4
326
5 9 .0
1 35 1
111.5
7 74
5 5 .9
7 6 .0
material were included in the statistical analysis. Practice E691
Practice E691
was followed for the design and analysis of the data; the details
are given in Research Report No. RR:D01-1147.
NOTE 11—Whe
11—When
n tes
testin
ting
g in a spe
specifi
cificc loc
locatio
ation,
n, the hig
highes
hestt res
result
ultss
obtained may be the most representative. The most common errors made
during the testing process lead to artificially lower results, typically not
higher results. Characterizing a test area based on an apparent low or high
individual result should be done with caution.
NOTE 13—The pull-off strength of two of the coatings, identified during
the round robin as Coating A and Coating F, exceeded the measurement
limits of the testers with the accessories available at the time of testing,
and were theref
therefore
ore elimin
eliminated
ated from the statistical analysis.
9.1.9.
9.1
.9.2
2 If correctio
corrections
ns of the res
results
ults have been made, or if
certain values have been omitted such as the lowest or highest
values or others, reasons for the adjustments and criteria used.
9.1.9.3
9.1.9
.3 For any test where scoring was employed,
employed, indicate it
by pl
plac
acin
ing
g a fo
foot
otno
note
te su
supe
pers
rscr
crip
iptt be
besi
side
de eac
each
h da
data
ta po
poin
intt
affected and a footnote to that effect with information of the
scoring apparatus used at the bottom of each page on which
such data appears. Note any other deviations from the procedure.
9.1.9.4
9.1.9
.4 Note any other deviations from the procedure.
procedure.
10.1.1 Repeatability— Two
Two test results obtained within one
laboratory shall be judged not equivalent if they differ by more
than
th
an th
thee “r ” va
valu
luee fo
forr th
that
at ma
mate
teri
rial
al;; “r ” is th
thee in
inte
terv
rval
al
representing the critical difference between two test results for
the same material, obtained by the same operator using the
same equipment on the same day in the same laboratory.
10.1.1.1
10.1.
1.1 Repeatab
Repeatability
ility limits are listed in Tables
in Tables 1-5.
1-5.
10.1.2 Reproducibility— Two
Two test results shall be judged not
equivalent if they differ by more than the “ R” value for that
material;
materia
l; “ R” is the int
interv
erval
al rep
repres
resent
enting
ing the dif
differ
ferenc
encee between
tw
een tw
two
o te
test
st re
resu
sults
lts fo
forr th
thee sa
same
me ma
mate
teri
rial,
al, ob
obta
tain
ined
ed by
different operators using different equipment in different laboratories.
10.1.2.1
10.1.
2.1 Reprod
Reproducibili
ucibility
ty limits are listed in Tables
in Tables 1-5.
1-5.
10.1.3
10.
1.3 Any judgment
judgment in acco
accorda
rdance
nce with the
these
se two sta
statetements would have an approximate 95 % probability of being
correct.
NOTE 12—Us
12—Usee cau
cautio
tion
n wit
with
h sta
statis
tistica
ticall ana
analys
lysis
is of dat
data,
a, suc
such
h as
averaging of results, for test results that include glue failure, termination
of the test, or exceeding the capacity of the test equipment. The reported
load for these types of test results are not representative of the maximum
load capacity of the coating tested.
10. Pre
Precisi
cision
on and Bias5
10.1
10
.1 The pr
prec
ecis
isio
ion
n of th
this
is te
test
st me
meth
thod
od is ba
base
sed
d on an
interlabor
interla
borato
atory
ry stu
study
dy of Test Met
Method
hod D45
D4541
41 con
conduc
ducted
ted in
6
2006, using the parameters of Test Method D4541-09. Analysts
lys
ts fro
from
m sev
seven
en lab
labora
orator
tories
ies test
tested
ed six dif
differ
ferent
ent coa
coating
tingss
applied to 1 ⁄ 4 in. thick hot-rolled carbon steel plates using five
differ
dif
ferent
ent adh
adhesi
esion
on tes
testers
ters.. Eve
Every
ry “tes
“testt res
result
ult”” rep
repres
resent
entss an
individual determination. In order to standardize and balance
the data, any pull which exceeded the tester’s upper limit with
the available accessories at the time of testing was eliminated
from the statistical analysis. Any pull in which there was 50 %
or more glue fracture was also eliminated from the statistical
analysis. If four valid pulls were obtained from one operator
for a given material, the fourth was eliminated and the first
three valid replicate test results (from one operator) for each
10.2 Bias— At
At the time of the study, there was no accepted
reference material suitable for determining the bias for this test
method, therefore no statement is being made.
10.3 The precision statement
statement was determ
determined
ined through
through statistical examination of 394 results, produced by analysts from
seven
sev
en lab
labora
orator
tories,
ies, on fou
fourr coa
coatin
tings,
gs, usi
using
ng five dif
differ
ferent
ent
inst
in
stru
rume
ment
nts.
s. Di
Difffe
fere
rent
nt co
coati
ating
ngss we
were
re us
used
ed as a me
mean
anss to
achievee a range of pull-o
achiev
pull-offf streng
strengths
ths covering the opera
operating
ting
range of all the instruments.
10.3.1
10.3.
1 Results obtained
obtained by the same operator
operator using instruments from the same Method should be considered suspect if
they differ
differ in percent relative by more than the Intral
Intralaborat
aboratory
ory
values given in Table
in Table 6.
6. Triplicate results obtained by different
operators using instruments from the same Method should be
considered suspect if they differ in percent relative by more
than the Interlaboratory values given in Table 6.
6.
5
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D01-1147. Contact ASTM Customer
Service at
6
Scotch Weld
Weld 420, available from 3M, Adhesives, Coatings and Sealers Div., 3M
Center, St. Paul, MN 55144, was used in the Interlaboratory Study round robin.
6
D4541 − 17
TABLE 2 Adhesion Testing Method C, Pull-Off Strength ( psi )
Repeatability Reproducibility
Standard
Standard
Deviation
Deviation
x¯
sr
sR
B
1 9 74
26 1
32 4
C
1 2 21
13 6
54 8
D
2110
25 2
31 6
E
2012
20
23 9
35 9
Repeatability
Coating
Coatin
g Avera
Average
ge
Limit
x¯
r
% of average
B
1 9 74
73 2
3 7 .1
C
1 2 21
38 2
3 1 .3
D
2110
70 6
3 3 .5
E
2 0 12
66 9
3 3 .3
Avg.
3 0 .4
Coating
Coatin
g Avera
Average
ge
Repeatability
Limit
TABLE 4 Adhesion Testing Method E, Pull-Off Strength ( psi )
Repeatability Reproducibility
Standard
Standard
Deviation
Deviation
x¯
sr
sR
B
2 21 0
17 3
2 15
C
1120
115
1 55
D
2 48 1
24
36 1
4 22
E
2 44 9
17 3
1 98
Repeatability
Coating
Coatin
g Avera
Average
ge
Limit
x¯
r
% of average
B
2 21 0
48 3
2 1. 9
C
1120
32 1
2 8. 7
D
2 48 1
1011
4 0 .7
E
2 44 9
48 5
1 9. 8
Avg.
2 7 .8
Reproducibility
Limit
Coating
Coatin
g Avera
Average
ge
r
R
7 32
9 07
3 82
15 35
7 06
8 86
6 69
10 04
Reproducibility
Limit
R
% of average
907
4 5 .9
15 35
1 2 5 .7
886
4 2 .0
10 04
4 9 .9
7 0. 5
TABLE 3 Adhesion Testing Method D, Pull-Off Strength ( psi )
Repeatability Reproducibility
Standard
Standard
Deviation
Deviation
x¯
sr
sR
B
2 4 58
14 6
27 0
C
1 2 32
31
116
D
2 7 07
15 5
23 3
E
2 3 54
16 3
27 3
Repeatability
Coating
Coatin
g Avera
Average
ge
Limit
x¯
r
% of average
B
2 4 58
40 8
1 6 .6
C
1 2 32
87
7 .1
D
2 7 07
43 4
1 6 .0
E
2 3 54
45 6
1 9 .4
Avg.
1 4 .8
Coating
Coatin
g Avera
Average
ge
Repeatability
Limit
Repeatability
Limit
Reproducibility
Limit
r
SR
4 83
60 1
3 21
43 3
1011
1181
4 85
55 5
Reproducibility
Limit
R
% of average
6 01
2 7. 2
4 33
3 8. 7
1181
4 7. 6
5 55
2 2. 7
3 4. 1
TABLE 5 Adhesion Testing Method F, Pull-Off Strength ( psi )
Repeatability Reproducibility
Standard
Standard
Deviation
Deviation
x¯
sr
sR
B
2 07 0
10 2
1 25
C
1106
60
1 08
D
2 36 8
12 4
1 60
E
2 32 7
21 7
2 37
Repeatability
Coating
Coatin
g Avera
Average
ge
Limit
x¯
r
% of average
B
2 07 0
28 7
1 3. 9
C
1106
16 9
1 5. 3
D
2 36 8
34 7
1 4. 7
E
2 32 7
60 9
2 6. 2
Avg.
1 7 .5
Reproducibility
Limit
Coating
Coatin
g Avera
Average
ge
r
SR
4 08
7 55
87
324
4 34
6 51
4 56
7 64
Reproducibility
Limit
R
% of average
7 55
3 0 .7
32 4
2 6. 3
6 51
2 4 .0
7 64
3 2 .5
2 8 .4
11.. Keywo
11
Keywords
rds
11.1
11
.1 adhesi
adhesion;
on; coatings; field; metal subst
substrates;
rates; paint; portable; pull-off strength; tensile test
7
Repeatability
Limit
Reproducibility
Limit
r
SR
28 7
3 51
1 69
304
34 7
4 49
60 9
6 64
Reproducibility
Limit
R
% of average
35 1
1 7. 0
30 4
2 7. 5
44 9
1 9. 0
66 4
2 8. 5
2 3. 0
D4541 − 17
TABLE 6 Precision of Adhesion Pull-Off Measurements (averaged
across coating types for each instrument)
instrument)
Intralaboratory
M e th o d B
M e th o d C
M e th o d D
M e th o d E
M e th o d F
Maximum
Recommended
Difference, %
6 4 .7
3 3 .8
1 4 .8
2 7 .8
1 7 .5
Interlaboratory
M e th o d B
M e th o d C
M e th o d D
M e th o d E
M e th o d F
Maximum
Recommended
Difference, %
7 6. 0
6 5. 9
2 8. 4
3 4. 1
2 3 .0
ANNEXES
(Mandatory Information)
A1. FIXED-ALIGN
FIXED-ALIGNMENT
MENT ADHESION
ADHESION TESTER TYPE II (TEST METHOD B)
A1.1 Apparatus:
A1.2.1
A1.2
.1 Cente
Centerr th
thee be
bear
arin
ing
g ri
ring
ng on th
thee co
coat
atin
ing
g su
surf
rface
ace
concentric with the loading fixture. Turn the hand wheel or nut
of the tester counterclock
counterclockwise,
wise, lowering
lowering the grip so that it slips
under the head of the loading fixture.
A1.1.1 This is a fixed-alignment portable
portable tester, as shown
shown in
7,8
Fig. A1.1.
A1.1.
NOTE A1.1—Precision data for Type II instruments shown in Table 6
were obtained using the devices described in Fig.
in Fig. A1.1.
A1.1.
A1.2.2 Align or shim the three instrument swivel pads of the
tripod base so that the instrument will pull perpendicularly to
the surface at the bearin
bearing
g ring. The annular ring can be used on
flexible substrates.
A1.1.2 The
The test
tester
er is com
compri
prised
sed of det
detach
achabl
ablee alu
alumin
minum
um
loading fixtures having a flat conic base that is 20 mm (0.8 in.)
in di
diam
amete
eterr on on
onee en
end
d fo
forr sec
secur
urin
ing
g to th
thee co
coat
atin
ing,
g, an
and
d a
circu
cir
cula
larr TT-bo
bolt
lt he
head
ad on th
thee ot
othe
herr en
end,
d, a ce
cent
ntra
rall gr
grip
ip fo
for
r
engaging the loading fixture that is forced away from a tripod
base by the interaction of a hand wheel (or nut), and a coaxial
bolt
bo
lt co
conn
nnect
ected
ed th
thrrou
ough
gh a se
seri
ries
es of be
belle
llevil
ville
le wa
wash
sher
ers,
s, or
springs in later models, that acts as both a torsion relief and a
spring that displaces a dragging indicator with respect to a
scale.
A1.2.3 Take up the slack between the various members
members and
slide the dragging (force) indicator located on the tester to zero.
A1.2.4
A1.
2.4 Fir
Firmly
mly hold the ins
instru
trumen
mentt wit
with
h one hand.
hand. Do not
allow the base to move or slide during the test. With the other
hand,
han
d, tur
turn
n the hand whe
wheel
el clo
clockw
ckwise
ise usi
using
ng as smo
smooth
oth and
constant motion as possible. Do not jerk or exceed a stress rate
of 150 psi/s (1 MPa/s) that is attained by allowing in excess of
7 s/7 MPa (7 s/1000 psi), stress. If the 14 or 28 MPa (2000 or
4000 psi) models are used, the hand wheel is replaced with a
nut requiring a wrench for tightening. The wrench must be used
in a plane parallel to the substrate so that the loading fixture
will not be removed by a shearing force or misalignment, thus
negatin
neg
ating
g the res
result
ults.
s. The max
maximu
imum
m loa
load
d mus
mustt be rea
reache
ched
d
within about 100 s.
A1.1.3 The force is indicated by measuring the maximum
A1.1.3
spring displacement when loaded. Care should be taken to see
that substrate bending does not influence its final position or
the actual force delivered by the spring arrangement.
A1.1.4 The devices are available
A1.1.4
available in four ranges:
ranges: From 3.5,
7.0, 14, and 28 MPa (0 to 500, 0 to 1000, 0 to 2000, and 0 to
4000 psi).
A1.2.5 The pulling
A1.2.5
pulling for
force
ce app
applied
lied to the loading
loading fixt
fixture
ure is
increased to a maximum or until the system fails at its weakest
locus.
loc
us. Upo
Upon
n fra
fractur
cture,
e, the sca
scale
le will rise slig
slightl
htly
y, whi
while
le the
draggi
dra
gging
ng ind
indicat
icator
or reta
retains
ins the app
appare
arent
nt loa
load.
d. The app
appara
aratus
tus
scale
sca
le ind
indicat
icates
es an app
approx
roximat
imatee loa
load
d dir
directl
ectly
y in pou
pounds
nds per
square inch, but may be compared to a calibration curve.
A1.2 Procedure:
7
The sole source of supply of the Elcometer, Model 106, adhesion tester known
to the committee at this time is Elcometer Instruments, Ltd., Edge Lane, Droylston,
Manchester M35 6UB, United Kingdom, England.
8
If you are aware of alternative suppliers, please provide this information to
ASTM Headquarters. Your comments will receive careful consideration at a meeting
of the responsible technical committee,1 which you may attend
A1.2.6 Record the highest
highest value attained by readin
reading
g along
the bottom of the dragging indicator.
8
D4541 − 17
(a)
(b)
FIG. A1.1 Photograph (a) and Schematic (b) of Type II, Fixed Alignment Pull-Off Tester
9
D4541 − 17
A2. SELF-ALIGNIN
SELF-ALIGNING
G ADHESION TESTER
TESTER TYPE III (TEST METHOD C)
A2.1 Apparatus:
A2.1.5 The testers are available in three standard
standard working
ranges: 0 to 10 MPa (0 to 1500 psi), 0 to 15 MPa (0 to 2250
psi), 0 to 20 MPa (0 to 3000 psi). Special loading fixtures
shaped to test tubular sections are available.
A2.1.1
A2.1
.1 This
This is a se
self
lf-a
-alig
ligni
ning
ng te
teste
sterr, as sh
show
own
n in Fig.
9,8
A2.1..
A2.1
NOTE A2.1—Precision data for Type III instruments shown in Table
in Table 6
were obtained using the devices described in Fig.
in Fig. A2.1.
A2.1.
A2.2 Procedure:
A2.2.1 Follo
Follow
w the gener
general
al procedures
procedures described in Sections
6 and
and 7
7.. Procedures specific to this instrument are described in
this section
section..
A2.1.2 Loa
A2.1.2
Load
d is app
applied
lied through
through the center of the loading
loading
fixture by a hydraulic piston and pin. The diameter of the piston
bore is sized so that the area of the bore is equal to the net area
of the loading fixture. Therefore, the pressure reacted by the
loading fixture is the same as the pressure in the bore and is
transmitted directly to a pressure gauge.
A2.2.2 Inser
Insertt a decreas
decreased
ed TFE-fluorocarb
TFE-fluorocarbon
on plug into the
loading fixture until the tip protrudes from the surface of the
loadin
loa
ding
g fixt
fixture
ure.. Whe
When
n app
applyin
lying
g glu
gluee to the load
loading
ing fixt
fixture
ure,,
avoid getting glue on the plug. Remove plug after holding the
loading fixture in place for 10 s.
A2.1.3
A2.1.
3 The apparatus
apparatus is comprised of: a loading fixture,
fixture, 19
mm (0
(0.7
.75
5 in
in.)
.) ou
outs
tsid
idee di
diam
amete
eterr, 3 mm (0
(0.1
.125
25 in
in.)
.) in
insi
side
de
diameter, hydraulic piston and pin by which load is applied to
the loading fixture, hose, pressure gauge, threaded plunger and
handle.
A2.2.3 Ensur
Ensuree that the black needle of the tester is reading
zero. Connect a test loading fixture to the head and increase the
pressure by turning the handle clockwise until the pin protrudes
from the loading fixture. Decrease pressure to zero and remove
the test loading fixture.
A2.1.4
A2.
1.4 The force is ind
indicat
icated
ed by the max
maximu
imum
m hyd
hydrau
raulic
lic
pressure as displayed on the gauge, since the effective areas of
the piston bore and the loading fixture are the same.
A2.2.4 Conne
Connect
ct the head to the loadin
loading
g fixture to be tested,
by pu
pulli
lling
ng ba
back
ck th
thee sn
snap
ap-o
-on
n ri
ring
ng,, pu
push
shin
ing
g th
thee he
head
ad an
and
d
releasing the snap-on ring. Ensure the tester is held normal to
the surface to be tested and that the hose is straight.
9
The sole source of supply of the Hate Mark VII adhesion tester known to the
committee at this time is Hydraulic Adhesion Test Equipment, Ltd., 629 Inlet Rd.,
North Palm Beach, FL 33408.
A2.2.5 Incre
Increase
ase the pressu
pressure
re slowly by turnin
turning
g the handle
clockwise until either the maximum load or fracture is reached.
10
D4541 − 17
(a)
(b)
FIG. A2.1 Photograph (a) and Schematic (b) of Type III, Self-Alignment Tester
11
D4541 − 17
A3. SELF-ALIGNME
SELF-ALIGNMENT
NT ADHESION TESTER
TESTER TYPE IV (TEST METHOD D)
A3.1 Apparatus:
A3.2.1 Follo
Follow
w the gener
general
al procedures
procedures described in Sections
6 and
and 7
7.. Procedures specific to Type IV testers are described in
the following section.
A3.1.1 This is a self-al
A3.1.1
self-aligning
igning automated
automated tester,
tester, which may
have a self-contained pressure source and has a control module
thatt co
tha
cont
ntro
rols
ls a ch
choi
oice
ce of dif
diffe
fere
rent
nt lo
load
ad ra
rang
ngee de
detac
tachi
hing
ng
assemblies, or pistons. It is shown in Fig. A3.1.
A3.1.
A3.2.2 Adher
Adheree a loadin
loading
g fixture to the coating based on the
epoxy manufacturer’s instructions, employing either a cut-off
ring or glue mask to reproducibly define the area being tested.
On lar
larger
ger size
sized
d loa
loadin
ding
g fixt
fixture
ures,
s, simp
simply
ly wip
wipee awa
away
y exc
excess
ess
epoxy with a cotton tipped applicator or rag.
NOTE A3.1—Precision data for Type IV instruments shown in Table 6
were obtained using the devices described in Fig.
in Fig. A3.1.
A3.1.
A3.1.2 The apparatus
A3.1.2
apparatus is comprised
comprised of: ( 1) a loading fixture,
(2) a detaching assembly, or piston, ( 3) one of several control
modules, and (4) a pressurized air source.
A3.2.3 Place the piston over the loading fixture
fixture and gently
thread the reaction plate (top of piston) onto the loading fixture.
A3.1.3
A3.1.
3 The loading fixtures
fixtures are availab
available
le on many different
different
sizes (3 to 75 mm) based on the particulars
particulars of the system being
tested.
test
ed. The sta
standa
ndard
rd loading
loading fixt
fixture
ure is 12.
12.5
5 mm (0.
(0.5
5 in) in
diameter. The face of the loading fixture can be rough, smooth,
curved, machined, etc.
A3.2.4 Attach the appropriate
appropriate pneumatic hoses and ensur
ensuree
that the control module has an air supply of at least 0.67 Mpa
(100 psi) as read on the supply gauge. Zero the Piston Pressure
gauge/display.
A3.2.5
A3.
2.5 Ensure
Ensure that the Rate Valv
alvee is clo
closed
sed (cl
(clock
ockwis
wisee
finger tight) and then press and hold the Run button. Slowly
open the Rate Valve (counterclockwise) and monitor the Piston
Pressure gauge/display to obtain a rate of pressure increase of
less than 1 MPa/s (100 psi/s) yet allowing for the entire test to
be complete within 100 s. When the loading fixture detaches
from the surface or the required pressure is attained, release the
Run button.
A3.1.4 The pis
A3.1.4
piston
tonss are als
also
o ava
availab
ilable
le in sev
severa
erall dif
differ
ferent
ent
sizes, or load ranges. It is recommended that a piston is chosen
so th
that
at th
thee mi
midp
dpoi
oint
nt of th
thee ra
rang
ngee is clo
close
se to th
thee su
susp
spec
ected
ted
tensile strength of the coating to be tested. This will provide the
most forgiveness in errors of assumed coating strength.
A3.1.5 Sev
A3.1.5
Severa
erall mod
models
els of con
contro
troll mod
module
uless are ava
availab
ilable.
le.
The digital models may include optional accessories allowing
for features such as wireless real-time transmission of pull-tests
via Bluetooth and your PC, LabVIEW-created software, USB
camera attachment to photo document your pulls, and computer generated reporting capabilities.
A3.2.6
A3.
2.6 Ope
Open
n the Rate Valv
alvee eve
even
n fur
further
ther (co
(count
unterc
erclock
lock-wise) to relieve the residual pressure so the loading fixture can
be removed from the piston to prepare for the next test.
A3.2.7 Record both
both the maximum pressure
pressure attained and the
specific piston used. Convert the maximum Piston Pressure to
the load applied to the coating using the conversion charts or
set the specific testing parameters within the software to have
this step completed automatically.
A3.1.6
A3.1
.6 The
The pr
press
essur
uriz
ized
ed air so
sour
urce
ce ma
may
y be ( 1) a self
lf-contained miniature air cylinder for maximum portability, ( 2)
shop (bottled) air, or ( 3) air from an automated pump.
A3.2 Procedure:
12
D4541 − 17
(a)
FIG. A3.1 Photograph
Photograph (a) and Schematic of Piston (b) of Type IV Self-A
Self-Alignme
lignment
nt Adhesion Tester
Tester
13
D4541 − 17
A4. SELF-ALIGNIN
SELF-ALIGNING
G ADHESION TESTER
TESTER TYPE V (TEST METHOD E)
A4.1 Apparatus:
A4.2 Procedure:
A4.1.1
A4.1
.1 This
This is a se
self
lf-a
-alig
ligni
ning
ng te
teste
sterr, as sh
show
own
n in Fig.
10,8
A4.1..
A4.1
A4.2.1 Follo
Follow
w the gener
general
al procedures
procedures described in Sections
6 and
and 7
7.. Procedures specific to Type V Testers are described in
this section
section..
NOTE A4.1—Precision data for Type V instruments shown in Table
in Table 6
were obtained using the devices described as “Manual” in Fig.
in Fig. A4.1.
A4.1.
A4.2.2
A4.2
.2 En
Ensu
sure
re th
thee pr
pres
essu
sure
re re
relie
lieff va
valv
lvee on th
thee pu
pump
mp is
completely open. Push the actuator handle completely down
into the actuator assembly.
A4.1.2 A self-a
A4.1.2
self-alignin
ligning
g spherical loading
loading fixture head is used
by this tester. Load evenly distributes pulling force over the
surface being tested, ensuring a perpendicular, balanced pulloff. A loading fixture of 20 mm (0.78 in.) is equal to the area
of the pos
positio
ition
n bor
boree in the actu
actuato
atorr. The
Theref
refore
ore,, the pre
pressu
ssure
re
reacted by the loading fixture is the same as the pressure in the
actuator and is transmitted directly to the pressure gauge. The
tester performs automatic conversion calculations for the 50
mm (1.97 in.) loading fixtures and other common sizes of 10
and 14 mm (0.39 in. and 0.55 in. respectively).
A4.2.3 Place the actuator assembly
assembly over the loading fixture
head and attach the quick coupling to the loading fixture. Close
the pressure relief valve on the pump. Select the appropriate
loadin
loa
ding
g fixt
fixture
ure size on the dis
displa
play
y and then press the zer
zero
o
button.
A4.1.4
A4.
1.4 The dis
display
play on the pre
pressu
ssure
re gau
gauge
ge ind
indicat
icates
es the
maximum force and the rate of pull.
A4.2.4 Pri
A4.2.4
Prime
me the pump by pum
pumpin
ping
g the handle
handle unt
until
il the
displa
dis
played
yed rea
readin
ding
g app
approa
roache
chess the pri
primin
ming
g pre
pressu
ssure
re as explained in the instruction manual. Return the pump handle to
its full upright position and then complete a single stroke at a
uniform rate of no more than 1 MPa/s (150 psi/s) as shown on
the display until the actuator pulls the loading fixture from the
surface.
A4.1.5 The tester is available with accessories
A4.1.5
accessories for finishes
on plastics, metals, and wood. Special loading fixtures, typically 10 mm (0.39 in.) and 14 mm (0.55 in.) are available for
use on curved surfaces and when higher pull-off pressures are
required.
A4.2.5 Immed
Immediately
iately following
following the pull, open the press
pressure
ure
relief valve on the pump to release the pressure. The display
will maintain the maximum pressure reading. Record this pull
offf pre
of
pressu
ssure
re into the tes
tester’
ter’ss mem
memory
ory and mar
mark
k the loa
loadin
ding
g
fixture for future qualitative analysis.
A4.1.3
A4.1.
3 The apparatus
apparatus is comprised of: a loading fixture,
fixture, 10
to 50 mm (0.39 and 1.97 in. respectively) diameter, hydraulic
actuator by which the load is applied to the loading fixture,
pressure gauge with LCD display, and hydraulic pump.
A4.2.6 A versio
version
n of this tester is available
available with an automatic
automatic
hydraulic pump.
10
The sole sou
source
rce of sup
supply
ply of the Pos
PosiT
iTest
est Pull-Off
Pull-Off Tester
Tester kno
known
wn to the
committee at this time is DeFelsko Corporation, 802 Proctor Avenue, Ogdensburg,
NY 13669 USA.
14
D4541 − 17
(a)
(b)
FIG. A4.1 Photograph (a) and Schematic (b) of Type V, Self-Aligning Tester
15
D4541 − 17
A5. SELF-ALIGNIN
SELF-ALIGNING
G ADHESION TESTER
TESTER TYPE VI (TEST METHOD F)
A5.1 Apparatus:
NOTE A5.1—Precision data for Type VI instruments shown in Table 6
were obtained using the devices described in Fig.
in Fig. A5.1.
A5.1.
A5.2.2 Ens
A5.2.2
Ensure
ure that the pressure
pressure in the pull mech
mechani
anism
sm is
released by opening the valve at the bottom of the cylinder.
Turn
Tu
rn the dra
draggi
gging
ng indicator
indicator to zer
zero
o in lin
linee wit
with
h the gauge
indicator needle.
A5.1.2
A5.
1.2 The self
self-al
-align
igning
ing test
testing
ing hea
head
d use
usess fou
fourr ind
indepe
epenndently operated feet to ensure that the pull stress on the loading
fixture is evenly distributed independently of the shape of the
substrate or the angle of the loading fixture to the surface. See
Fig. A5.1
A5.2.3
A5.
2.3 Att
Attach
ach the self
self-ali
-aligni
gning
ng test hea
head
d to the hyd
hydrau
raulic
lic
cable mechanism
mechanism using the quick release connector on the side
of the test head. Return the crank handle to the start position
and ensure that the four pistons of the self-aligning head are
level by pushing the head against a flat surface.
A5.1.1
A5.1.
1 This is a self-a
self-alignin
ligning
g tester, as shown in Fig.
in Fig. A5.1.
A5.1.
A5.1.3 The apparatus
A5.1.3
apparatus comprises
comprises a crank handle
handle pull mechanism with a hydraulic cable mechanism, a self-aligning test
head rated at 6.3 kN and loading fixtures.
A5.2.4 Place the rel
A5.2.4
releva
evant
nt sup
suppor
portt rin
ring
g ove
overr the loa
loadin
ding
g
fixture.
fixtur
e. A suppo
support
rt ring is not required
required for 25 mm, 50 mm, or 70
mm diameter loading fixtures or for 50 mm square loading
fixtures.
A5.1.4
A5.1
.4 A ra
rang
ngee of lo
load
adin
ing
g fix
fixtu
ture
res,
s, fr
from
om 2.
2.8
8 to 70 mm
diameter is available. The 20 mm diameter loading fixtures are
directly connected to the test head by means of a quick release
connector. Other loading fixture sizes are supplied with threads
machined to allow connection to the self-aligning test head
using an adapter. Loading fixtures with diameters in the range
2.8 to 5.7 mm are used with a micro self-aligning test head
rated at 1 kN.
A5.2.5 Attach the test head to the loading
A5.2.5
loading fixt
fixture
ure either
either
directl
dir
ectly
y or usi
using
ng the ada
adapte
pter,
r, whe
where
re app
approp
ropriat
riate.
e. Clos
Closee the
valve.
A5.2.6 Ens
A5.2.6
Ensure
ure that the hydrauli
hydraulicc cab
cable
le mec
mechan
hanism
ism is not
pulled tight. Hold the pull mechanism in one hand and operate
the crank with the other using a smooth and regular motion to
ensuree that the force is applie
ensur
applied
d evenly until the desire
desired
d value is
reached or the fracture occurs.
A5.1.5 The force applied to the loading fixture is displayed
A5.1.5
displayed
on a hydraulic pressure gauge with a dragging indicator that
shows the maximum reading at the point where the loading
fixture is removed from the surface. The gauge carries both PSI
and MPa values on two scales.
A5.2.7 Immed
Immediately
iately following
following the comple
completion
tion of the pull,
open the valve to release any residual pressure and return the
crank handle
handle to the start position. The unit is now ready for the
next pull.
A5.2 Procedure:
A5.2.8 Note the value indicated by the dragg
dragging
ing indicator
and mark the loading fixture for further analysis as described in
Section 8.
A5.2.1 Follow
A5.2.1
Following
ing the gener
general
al procedures described
described in Sections 6 and 7, proced
procedure
uress spe
specific
cific to Type VI test
testers
ers are
described in the following section.
16
D4541 − 17
(a)
(b)
FIG. A5.1 Photograph (a) and Schematic (b) of Type VI, Self-Aligning Tester
17
D4541 − 17
SUMMARY OF CHANGES
Committ
Comm
ittee
ee D0
D01
1 ha
hass id
iden
enti
tified
fied th
thee lo
loca
catio
tion
n of sel
select
ected
ed ch
chan
ange
gess to th
this
is st
stan
anda
dard
rd sin
since
ce th
thee las
lastt is
issu
suee
1
(D4541-09 ) that may impact the use of this standard. (Approved August 1, 2017.)
ɛ
(1) TBD
ASTM International
International takes no positi
position
on respecting the validi
validity
ty of any patent rights assert
asserted
ed in connec
connection
tion with any item mentio
mentioned
ned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible
respon
sible technical
technical committee, which you may attend. If you feel that your comments have not receiv
received
ed a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.
This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address
addr
ess or at 610610-832832-9585
9585 (pho
(phone),
ne), 610610-832832-9555
9555 (fax
(fax),
), or serv
service@
ice@astm
astm.org
.org (e-m
(e-mail)
ail);; or thro
through
ugh the ASTM webs
website
ite
(www.astm.
(www
.astm.org).
org). Permission
Permission rights to photocopy the standa
standard
rd may also be secure
secured
d from the Copyri
Copyright
ght Clearance Center,
Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; />
18