Designation: D4541 − 09´1

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 adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

ε1 NOTE—Practice D3980 was deleted from Section 2 in August 2010.

1. Scope* sion bonds between the loading fixture and the specimen
1.1 This test method covers a procedure for evaluating the surface or the cohesive strengths of the adhesive, coating
pull-off strength (commonly referred to as adhesion) of a layers, and substrate.
coating system from metal substrates. Pull-off strength of 1.4 This test can be destructive and spot repairs may be
coatings from concrete is described in Test Method D7234. The necessary.
test determines either the greatest perpendicular force (in 1.5 The values stated in MPa (inch-pound) units are to be
tension) that a surface area can bear before a plug of material regarded as the standard. The values given in parentheses are
is detached, or whether the surface remains intact at a pre- for information only.
scribed force (pass/fail). Failure will occur along the weakest
plane within the system comprised of the test fixture, adhesive, 1.6 This standard does not purport to address all of the
coating system, and substrate, and will be exposed by the safety concerns, if any, associated with its use. It is the
fracture surface. This test method maximizes tensile stress as responsibility of the user of this standard to establish appro-
compared to the shear stress applied by other methods, such as priate safety and health practices and determine the applica-
scratch or knife adhesion, and results may not be comparable. bility of regulatory limitations prior to use.
NOTE 1—The procedure in this standard was developed for metal 2. Referenced Documents
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 2.1 ASTM Standards:3
be addressed by the user/specifier. D2651 Guide for Preparation of Metal Surfaces for Adhesive
1.2 Pull-off strength measurements depend upon both ma- Bonding
terial and instrumental parameters. Results obtained by each D3933 Guide for Preparation of Aluminum Surfaces for
test method may give different results. Results should only be Structural Adhesives Bonding (Phosphoric Acid Anodiz-
assessed for each test method and not be compared with other ing)
instruments. There are five instrument types, identified as Test D7234 Test Method for Pull-Off Adhesion Strength of Coat-
Methods B-F. It is imperative to identify the test method used ings on Concrete Using Portable Pull-Off Adhesion Tes-
when reporting results. ters
NOTE 2—Method A, which appeared in previous versions of this E691 Practice for Conducting an Interlaboratory Study to
standard, has been eliminated as its main use is for testing on concrete Determine the Precision of a Test Method
substrates (see Test Method D7234).
2.2 ANSI Standard:
1.3 This test method uses a class of apparatus known as N512 Protective Coatings (Paints) for the Nuclear Industry4
portable pull-off adhesion testers.2 They are capable of apply- 2.3 ISO Standard:
ing a concentric load and counter load to a single surface so ISO 4624 Paints and Varnish—Pull-Off Test for Adhesion4
that coatings can be tested even though only one side is
accessible. Measurements are limited by the strength of adhe- 3. Summary of Test Method
3.1 The general pull-off test is performed by securing a
loading fixture (dolly, stud) normal (perpendicular) to the
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
and Related Coatings, Materials, and Applications and is the direct responsibility of
3
Subcommittee D01.46 on Industrial Protective Coatings. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Feb. 1, 2009. Published April 2009. Originally contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
approved in 1993. Last previous edition approved in 2002 as D4541 – 02. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D4541-09E01. the ASTM website.
2 4
The term adhesion tester may be somewhat of a misnomer, but its adoption by Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
two manufacturers and at least two patents indicates continued usage. 4th Floor, New York, NY 10036, http://www.ansi.org.

*A Summary of Changes section appears at the end of this standard

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 D4541 − 09´1
surface of the coating with an adhesive. After the adhesive is 5.2 Solvent, or other means for cleaning the loading fixture
cured, a testing apparatus is attached to the loading fixture and surface. Finger prints, moisture, and oxides tend to be the
aligned to apply tension normal to the test surface. The force primary contaminants.
applied to the loading fixture is then gradually increased and 5.3 Fine Sandpaper, or other means of cleaning the coating
monitored until either a plug of material is detached, or a that will not alter its integrity by chemical or solvent attack. If
specified value is reached. When a plug of material is detached, any light sanding is anticipated, choose only a very fine grade
the exposed surface represents the plane of limiting strength abrasive (400 grit or finer) that will not introduce flaws or leave
within the system. The nature of the failure is qualified in a residue.
accordance with the percent of adhesive and cohesive failures,
and the actual interfaces and layers involved. The pull-off 5.4 Adhesive5, for securing the fixture to the coating that
strength is computed based on the maximum indicated load, does not affect the coating properties. Two component epoxies
the instrument calibration data, and the original surface area and acrylics have been found to be the most versatile.
stressed. Pull-off strength results obtained using different 5.5 Magnetic or Mechanical Clamps, if needed, for holding
devices may be different because the results depend on the fixture in place while the adhesive cures.
instrumental parameters (see Appendix X1). 5.6 Cotton Swabs, or other means for removing excess
adhesive and defining the adhered area. Any method for
4. Significance and Use removing excess adhesive that damages the surface, such as
4.1 The pull-off strength of a coating is an important scoring (see 6.7), must generally be avoided since induced
performance property that has been used in specifications. This surface flaws may cause premature failure of the coating.
test method serves as a means for uniformly preparing and 5.7 Circular Hole Cutter (optional), to score through to the
testing coated surfaces, and evaluating and reporting the substrate around the loading fixture.
results. This test method is applicable to any portable apparatus
meeting the basic requirements for determining the pull-off 6. Test Preparation
strength of a coating. 6.1 The method for selecting the coating sites to be prepared
4.2 Variations in results obtained using different devices or for testing depends upon the objectives of the test and
different substrates with the same coating are possible (see agreements between the contracting parties. There are,
Section 10). Therefore, it is recommended that the type of however, a few physical restrictions imposed by the general
apparatus and the substrate be mutually agreed upon between method and apparatus. The following requirements apply to all
the interested parties. sites:
4.3 The purchaser or specifier shall designate a specific test 6.1.1 The selected test area must be a flat surface large
method, that is, B, C, D, E, or F when calling out this standard. enough to accommodate the specified number of replicate tests.
The surface may have any orientation with reference to
5. Apparatus gravitational pull. Each test site must be separated by at least
the distance needed to accommodate the detaching apparatus.
5.1 Adhesion Tester, commercially available, or comparable The size of a test site is essentially that of the secured loading
apparatus specific examples of which are listed in Annex fixture. At least three replications are usually required in order
A1-Annex A5. to statistically characterize the test area.
5.1.1 Loading Fixtures, having a flat surface on one end that 6.1.2 The selected test areas must also have enough perpen-
can be adhered to the coating and a means of attachment to the dicular and radial clearance to accommodate the apparatus, be
tester on the other end. flat enough to permit alignment, and be rigid enough to support
5.1.2 Detaching Assembly (adhesion tester), having a cen- the counter force. It should be noted that measurements close
tral grip for engaging the fixture. to an edge may not be representative of the coating as a whole.
5.1.3 Base, on the detaching assembly, or an annular bearing
6.2 Since the rigidity of the substrate affects pull-off
ring if needed for uniformly pressing against the coating
strength results and is not a controllable test variable in field
surface around the fixture either directly, or by way of an
measurements, some knowledge of the substrate thickness and
intermediate bearing ring. A means of aligning the base is
composition should be reported for subsequent analysis or
needed so that the resultant force is normal to the surface.
laboratory comparisons. For example, steel substrate of less
5.1.4 Means of moving the grip away from the base in as than 3.2 mm (1⁄8 in.) thickness usually reduces pull-off strength
smooth and continuous a manner as possible so that a torsion results compared to 6.4 mm (1⁄4-in.) thick steel substrates.
free, co-axial (opposing pull of the grip and push of the base
along the same axis) force results between them. 6.3 Subject to the requirements of 6.1, select representative
5.1.5 Timer, or means of limiting the loading rate to 1 MPa/s test areas and clean the surfaces in a manner that will not affect
(150 psi/s) or less for a 20 mm loading fixture so that the test integrity of the coating or leave a residue. To reduce the risk of
is completed in about 100 s or less. A timer is the minimum glue failures, the surface of the coating can be lightly abraded
equipment when used by the operator along with the force to promote adhesion of the adhesive to the surface. If the
indicator in 5.1.6.
5.1.6 Force Indicator and Calibration Information, for 5
Scotch Weld 420, available from 3M, Adhesives, Coatings and Sealers Div., 3M
determining the actual force delivered to the loading fixture. Center, St. Paul, MN 55144, was used in the round robin.

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 D4541 − 09´1
surface is abraded, care must be taken to prevent damage to the 7.1.2 Test Method B — Fixed Alignment Adhesion Tester
coating or significant loss of coating thickness. Solvent clean Type II:
the area to remove particulates after abrading. Select a solvent 7.1.2.1 Operate the instrument in accordance with Annex
that does not compromise the integrity of the coating. A1.
6.4 Clean the loading fixture surface as indicated by the 7.1.3 Test Method C — Self-Alignment Adhesion Tester Type
apparatus manufacturer. Failures at the fixture-adhesive inter- III:
face can often be avoided by treating the fixture surfaces in 7.1.3.1 Operate the instrument in accordance with Annex
accordance with an appropriate ASTM standard practice for A2.
preparing metal surfaces for adhesive bonding. 7.1.4 Test Method D — Self-Alignment Adhesion Tester Type
IV:
NOTE 3—Guides D2651 and D3933 are typical of well-proven methods 7.1.4.1 Operate the instrument in accordance with Annex
for improving adhesive bond strengths to metal surfaces. A3.
6.5 Prepare the adhesive in accordance with the adhesive 7.1.5 Test Method E — Self-Alignment Adhesion Tester Type
manufacturer’s recommendations. Apply the adhesive to the V:
fixture or the surface to be tested, or both, using a method 7.1.5.1 Operate the instrument in accordance with Annex
recommended by the adhesive manufacturer. Be certain to A4.
apply the adhesive across the entire surface. Position fixture on 7.1.6 Test Method F — Self-Alignment Adhesion Tester Type
the surface to be tested. Carefully remove the excess adhesive VI:
from around the fixture. (Warning—Movement, especially 7.1.6.1 Operate the instrument in accordance with Annex
twisting, can cause tiny bubbles to coalesce into large holidays A5.
that constitute stress discontinuities during testing.) 7.2 Select an adhesion-tester with a detaching assembly
NOTE 4—Adding about 1 percent of #5 glass beads to the adhesive having a force calibration spanning the range of expected
assists in even alignment of the test fixture to the surface. values along with its compatible loading fixture. Mid-range
6.6 Based on the adhesive manufacturer’s recommendations measurements are usually the best, but read the manufacturer’s
and the anticipated environmental conditions, allow enough operating instructions before proceeding.
time for the adhesive to set up and reach the recommended 7.3 If a bearing ring or comparable device (5.1.3) is to be
cure. During the adhesive set and early cure stage, a constant used, place it concentrically around the loading fixture on the
contact pressure should be maintained on the fixture. Magnetic coating surface. If shims are required when a bearing ring is
or mechanical clamping systems work well, but systems employed, place them between the tester base and bearing ring
relying on tack, such as masking tape, should be used with care rather than on the coating surface.
to ensure that they do not relax with time and allow air to 7.4 Carefully connect the central grip of the detaching
intrude between the fixture and the test area. assembly to the loading fixture without bumping, bending, or
6.7 Scoring around the fixture violates the fundamental in otherwise prestressing the sample and connect the detaching
situ test criterion that an unaltered coating be tested. If scoring assembly to its control mechanism, if necessary. For nonhori-
around the test surface is employed, extreme care is required to zontal surfaces, support the detaching assembly so that its
prevent micro-cracking in the coating, since such cracks may weight does not contribute to the force exerted in the test.
cause reduced adhesion values. Scored samples constitute a 7.5 Align the device according to the manufacturer’s in-
different test, and this procedure should be clearly reported structions and set the force indicator to zero.
with the results. Scoring is only recommended for thicker-film
NOTE 6—Proper alignment is critical, see Appendix X1. If alignment is
coatings, that is, thicknesses greater than 500 µm (20 mils), required, use the procedure recommended by the manufacturer of the
reinforced coatings and elastomeric coatings. Scoring, if adhesion tester and report the procedure used.
performed, shall be done in a manner that ensures the cut is 7.6 Increase the load to the fixture in as smooth and
made normal to the coating surface and in a manner that does continuous a manner as possible, at a rate of 1 MPa/s (150
not twist or torque the test area and minimizes heat generated psi/s) or less for a 20 mm loading fixture so that the test is
and edge damage or microcracks to the coating and the completed in about 100 s or less.
substrate. For thick coatings it is recommended to cool the
coating and substrate during the cutting process with water 7.7 Record the force attained at failure or the maximum
lubrication. force applied.
7.8 If a plug of material is detached, label and store the
NOTE 5—A template made from plywood with a hole of the same size
fixture for qualification of the failed surface in accordance with
drilled through it has been found to be an effective method to limit
sideways movement of the drill bit. 8.3.
6.8 Note the approximate temperature and relative humidity 7.9 Report any departures from the procedure such as
during the time of test. possible misalignment, hesitations in the force application, etc.
8. Calculation or Interpretation of Results
7. Test Procedure
8.1 If instructed by the manufacturer, use the instrument
7.1 Test Methods: calibration factors to convert the indicated force for each test
7.1.1 Test Method A (discontinued). into the actual force applied.

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 D4541 − 09´1
8.2 Either use the calibration chart supplied by the manu- 9.1.2 Temperature and relative humidity and any other
facturer or compute the relative stress applied to each coating pertinent environmental conditions during the test period.
sample as follows: 9.1.3 Description of the apparatus used, including: appara-
X 5 4F/πd 2 (1) tus manufacturer and model number, loading fixture type and
dimensions, and bearing ring type and dimensions.
where: 9.1.4 Description of the test system, if possible, by the
X = greatest mean pull-off stress applied during a pass/fail indexing scheme outlined in 8.3 including: product identity and
test, or the pull-off strength achieved at failure. Both generic type for each coat and any other information supplied,
have units of MPa (psi), the substrate identity (thickness, type, orientation, etc.), and the
F = actual force applied to the test surface as determined in adhesive used.
8.1, and 9.1.5 Test results.
d = equivalent diameter of the original surface area stressed 9.1.5.1 Date, test location, testing agent.
having units of inches (or millimetres). This is usually 9.1.5.2 For pass/fail tests, stress applied along with the
equal to the diameter of the loading fixture. result, for example, pass or fail and note the plane of any
8.3 For all tests to failure, estimate the percent of adhesive failure (see 8.3 and ANSI N512).
and cohesive failures in accordance to their respective areas 9.1.5.3 For tests to failure, report all values computed in 8.2
and location within the test system comprised of coating and along with the nature and location of the failures as specified in
adhesive layers. A convenient scheme that describes the total 8.3, or, if only the average strength is required, report the
test system is outlined in 8.3.1 through 8.3.3. (See ISO 4624.) average strength along with the statistics.
9.1.5.4 If corrections of the results have been made, or if
NOTE 7—A laboratory tensile testing machine is used in ISO 4624. certain values have been omitted such as the lowest or highest
8.3.1 Describe the specimen as substrate A, upon which values or others, reasons for the adjustments and criteria used.
successive coating layers B, C, D, etc., have been applied, 9.1.5.5 For any test where scoring was employed, indicate it
including the adhesive, Y, that secures the fixture, Z, to the top by placing a footnote superscript beside each data point
coat. affected and a footnote to that effect at the bottom of each page
8.3.2 Designate cohesive failures by the layers within which on which such data appears. Note any other deviations from the
they occur as A, B, C, etc., and the percent of each. procedure.
8.3.3 Designate adhesive failures by the interfaces at which
they occur as A/B, B/C, C/D, etc., and the percent of each. 10. Precision and Bias6,7
8.4 A result that is very different from most of the results 10.1 The precision of this test method is based on an
may be caused by a mistake in recording or calculating. If interlaboratory study of Test Method D4541 conducted in
either of these is not the cause, then examine the experimental 2006. Analysts from seven laboratories tested six different
circumstances surrounding this run. If an irregular result can be coatings applied to 1⁄4 in. thick hot-rolled carbon steel plates
attributed to an experimental cause, drop this result from the using five different adhesion testers. Every “test result” repre-
analysis. However, do not discard a result unless there are valid sents an individual determination. In order to standardize and
nonstatistical reasons for doing so or unless the result is a balance the data, any pull which exceeded the tester’s upper
statistical outlier. Valid nonstatistical reasons for dropping limit with the available accessories at the time of testing was
results include alignment of the apparatus that is not normal to eliminated from the statistical analysis. Any pull in which there
the surface, poor definition of the area stressed due to improper was 50 % or more glue failure was also eliminated from the
application of the adhesive, poorly defined glue lines and statistical analysis. If four valid pulls were obtained from one
boundaries, holidays in the adhesive caused by voids or operator for a given material, the fourth was eliminated and the
inclusions, improperly prepared surfaces, and sliding or twist- first three valid replicate test results (from one operator) for
ing the fixture during the initial cure. Scratched or scored each material were included in the statistical analysis. Practice
samples may contain stress concentrations leading to prema- E691 was followed for the design and analysis of the data; the
ture fractures. details are given in Research Report No. D01–1147.
8.5 Disregard any test where glue failure represents more NOTE 8—The pull-off strength of two of the coatings, identified during
the round robin as Coating A and Coating F, exceeded the measurement
than 50 % of the area. If a pass/fail criterium is being used and
limits of the testers with the accessories available at the time of testing,
a glue failure occurs at a pull-off strength greater than the and were therefore eliminated from the statistical analysis.
criterium, report the result as “pass with a pull-off strength >
10.1.1 Repeatability—Two test results obtained within one
{value obtained}...”
laboratory shall be judged not equivalent if they differ by more
8.6 Further information relative to the interpretation of the than the “r” value for that material; “r” is the interval
test results is given in Appendix X1. representing the critical difference between two test results for

9. Report
6
9.1 Report the following information: Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D01-1094.
9.1.1 Brief description of the general nature of the test, such 7
Supporting data have been filed at ASTM International Headquarters and may
as, field or laboratory testing, generic type of coating, etc. be obtained by requesting Research Report RR:D01-1147.

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 D4541 − 09´1
TABLE 1 Adhesion Testing Method B, Pull-Off Strength (psi) TABLE 4 Adhesion Testing Method E, Pull-Off Strength (psi)
Repeatability Reproducibility Repeatability Reproducibility
Repeatability Reproducibility Repeatability Reproducibility
Coating Average Standard Standard Coating Average Standard Standard
Limit Limit Limit Limit
Deviation Deviation Deviation Deviation
x̄ sr sR r R x̄ sr sR r SR
B 1195 278 330 777 925 B 2210 173 215 483 601
C 549 109 117 305 326 C 1120 115 155 321 433
D 1212 412 483 1155 1351 D 2481 361 422 1011 1181
E 1385 192 276 537 774 E 2449 173 198 485 555
Repeatability Reproducibility Repeatability Reproducibility
Coating Average Coating Average
Limit Limit Limit Limit
x̄ r % of average R % of average x̄ r % of average R % of average
B 1195 777 69.1 925 77.4 B 2210 483 21.9 601 27.2
C 549 305 55.6 326 59.0 C 1120 321 28.7 433 38.7
D 1212 1155 95.3 1351 111.5 D 2481 1011 40.7 1181 47.6
E 1385 537 38.8 774 55.9 E 2449 485 19.8 555 22.7
Avg. 64.7 76.0 Avg. 27.8 34.1

TABLE 2 Adhesion Testing Method C, Pull-Off Strength (psi) TABLE 5 Adhesion Testing Method F, Pull-Off Strength (psi)
Repeatability Reproducibility Repeatability Reproducibility
Repeatability Reproducibility Repeatability Reproducibility
Coating Average Standard Standard Coating Average Standard Standard
Limit Limit Limit Limit
Deviation Deviation Deviation Deviation
x̄ sr sR r R x̄ sr sR r SR
B 1974 261 324 732 907 B 2070 102 125 287 351
C 1221 136 548 382 1535 C 1106 60 108 169 304
D 2110 252 316 706 886 D 2368 124 160 347 449
E 2012 239 359 669 1004 E 2327 217 237 609 664
Repeatability Reproducibility Repeatability Reproducibility
Coating Average Coating Average
Limit Limit Limit Limit
x̄ r % of average R % of average x̄ r % of average R % of average
B 1974 732 37.1 907 45.9 B 2070 287 13.9 351 17.0
C 1221 382 31.3 1535 125.7 C 1106 169 15.3 304 27.5
D 2110 706 33.5 886 42.0 D 2368 347 14.7 449 19.0
E 2012 669 33.3 1004 49.9 E 2327 609 26.2 664 28.5
Avg. 30.4 70.5 Avg. 17.5 23.0

TABLE 3 Adhesion Testing Method D, Pull-Off Strength (psi) 10.1.2.1 Reproducibility limits are listed in Tables 1-5.
Repeatability Reproducibility
10.1.3 Any judgment in accordance with these two state-
Repeatability Reproducibility ments would have an approximate 95 % probability of being
Coating Average Standard Standard
Limit Limit
Deviation Deviation correct.
x̄ sr sR r SR
B 2458 146 270 408 755 10.2 Bias—At the time of the study, there was no accepted
C 1232 31 116 87 324 reference material suitable for determining the bias for this test
D 2707 155 233 434 651
E 2354 163 273 456 764 method, therefore no statement is being made.
Repeatability Reproducibility
Coating Average
Limit Limit
10.3 The precision statement was determined through sta-
x̄ r % of average R % of average tistical examination of 394 results, produced by analysts from
B 2458 408 16.6 755 30.7 seven laboratories, on four coatings, using five different
C 1232 87 7.1 324 26.3
D 2707 434 16.0 651 24.0
instruments. Different coatings were used as a means to
E 2354 456 19.4 764 32.5 achieve a range of pull-off strengths covering the operating
Avg. 14.8 28.4 range of all the instruments.
10.3.1 Results obtained by the same operator using instru-
ments from the same Method should be considered suspect if
the same material, obtained by the same operator using the they differ in percent relative by more than the Intralaboratory
same equipment on the same day in the same laboratory. values given in Table 6. Triplicate results obtained by different
10.1.1.1 Repeatability limits are listed in Tables 1-5. operators using instruments from the same Method should be
10.1.2 Reproducibility—Two test results shall be judged not considered suspect if they differ in percent relative by more
equivalent if they differ by more than the “R” value for that than the Interlaboratory values given in Table 6.
material; “R” is the interval representing the difference be-
tween two test results for the same material, obtained by 11. Keywords
different operators using different equipment in different labo- 11.1 adhesion; coatings; field; metal substrates; paint; por-
ratories. table; pull-off strength; tensile test

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TABLE 6 Precision of Adhesion Pull-Off Measurements (averaged
across coating types for each instrument)
Maximum Maximum
Intralaboratory Recommended Interlaboratory Recommended
Difference, % Difference, %
Method B 64.7 Method B 76.0
Method C 33.8 Method C 65.9
Method D 14.8 Method D 28.4
Method E 27.8 Method E 34.1
Method F 17.5 Method F 23.0

ANNEXES

(Mandatory Information)

A1. FIXED-ALIGNMENT ADHESION TESTER TYPE II (TEST METHOD B)

A1.1 Apparatus: A1.2.1 Center the bearing ring on the coating surface
A1.1.1 This is a fixed-alignment portable tester, as shown in concentric with the loading fixture. Turn the hand wheel or nut
Fig. A1.1.8,9 of the tester counterclockwise, lowering the grip so that it slips
under the head of the loading fixture.
NOTE A1.1—Precision data for Type II instruments shown in Table 6
were obtained using the devices described in Fig. 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
A1.1.2 The tester is comprised of detachable aluminum
the surface at the bearing ring. The annular ring can be used on
loading fixtures having a flat conic base that is 20 mm (0.8 in.)
flexible substrates.
in diameter on one end for securing to the coating, and a
circular T-bolt head on the other end, a central grip for A1.2.3 Take up the slack between the various members and
engaging the loading fixture that is forced away from a tripod slide the dragging (force) indicator located on the tester to zero.
base by the interaction of a hand wheel (or nut), and a coaxial A1.2.4 Firmly hold the instrument with one hand. Do not
bolt connected through a series of belleville washers, or allow the base to move or slide during the test. With the other
springs in later models, that acts as both a torsion relief and a hand, turn the hand wheel clockwise using as smooth and
spring that displaces a dragging indicator with respect to a constant motion as possible. Do not jerk or exceed a stress rate
scale. of 150 psi/s (1 MPa/s) that is attained by allowing in excess of
A1.1.3 The force is indicated by measuring the maximum 7 s/7 MPa (7 s/1000 psi), stress. If the 14 or 28 MPa (2000 or
spring displacement when loaded. Care should be taken to see 4000 psi) models are used, the hand wheel is replaced with a
that substrate bending does not influence its final position or nut requiring a wrench for tightening. The wrench must be used
the actual force delivered by the spring arrangement. in a plane parallel to the substrate so that the loading fixture
will not be removed by a shearing force or misalignment, thus
A1.1.4 The devices are available in four ranges: From 3.5, negating the results. The maximum stress must be reached
7.0, 14, and 28 MPa (0 to 500, 0 to 1000, 0 to 2000, and 0 to within about 100 s.
4000 psi).
A1.2.5 The pulling force applied to the loading fixture is
A1.2 Procedure: increased to a maximum or until the system fails at its weakest
locus. Upon failure, the scale will rise slightly, while the
8
The sole source of supply of the Elcometer, Model 106, adhesion tester known
dragging indicator retains the apparent load. The apparatus
to the committee at this time is Elcometer Instruments, Ltd., Edge Lane, Droylston, scale indicates an approximate stress directly in pounds per
Manchester M35 6UB, United Kingdom, England. square inch, but may be compared to a calibration curve.
9
If you are aware of alternative suppliers, please provide this information to
ASTM Headquarters. Your comments will receive careful consideration at a meeting A1.2.6 Record the highest value attained by reading along
of the responsible technical committee,1 which you may attend the bottom of the dragging indicator.

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 D4541 − 09´1

(a)

(b)

FIG. A1.1 Photograph (a) and Schematic (b) of Type II, Fixed Alignment Pull-Off Tester

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 D4541 − 09´1

A2. SELF-ALIGNING ADHESION TESTER TYPE III (TEST METHOD C)

A2.1 Apparatus: A2.1.5 The testers are available in three standard working
ranges: 0 to 10 MPa (0 to 1500 psi), 0 to 15 MPa (0 to 2250
A2.1.1 This is a self-aligning tester, as shown in Fig.
psi), 0 to 20 MPa (0 to 3000 psi). Special loading fixtures
A2.1.10,9
shaped to test tubular sections are available.
NOTE A2.1—Precision data for Type III instruments shown in Table 6
were obtained using the devices described in Fig. A2.1. A2.2 Procedure:
A2.1.2 Load is applied through the center of the loading A2.2.1 Follow the general procedures described in Sections
fixture by a hydraulic piston and pin. The diameter of the piston 6 and 7. Procedures specific to this instrument are described in
bore is sized so that the area of the bore is equal to the net area this section.
of the loading fixture. Therefore, the pressure reacted by the A2.2.2 Insert a decreased TFE-fluorocarbon plug into the
loading fixture is the same as the pressure in the bore and is loading fixture until the tip protrudes from the surface of the
transmitted directly to a pressure gauge. loading fixture. When applying adhesive to the loading fixture,
A2.1.3 The apparatus is comprised of: a loading fixture, 19 avoid getting adhesive on the plug. Remove plug after holding
mm (0.75 in.) outside diameter, 3 mm (0.125 in.) inside the loading fixture in place for 10 s.
diameter, hydraulic piston and pin by which load is applied to A2.2.3 Ensure that the black needle of the tester is reading
the loading fixture, hose, pressure gauge, threaded plunger and zero. Connect a test loading fixture to the head and increase the
handle. pressure by turning the handle clockwise until the pin protrudes
from the loading fixture. Decrease pressure to zero and remove
A2.1.4 The force is indicated by the maximum hydraulic the test loading fixture.
pressure as displayed on the gauge, since the effective areas of
the piston bore and the loading fixture are the same. A2.2.4 Connect the head to the loading fixture to be tested,
by pulling back the snap-on ring, pushing the head and
releasing the snap-on ring. Ensure the tester is held normal to
the surface to be tested and that the hose is straight.
10
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., A2.2.5 Increase the pressure slowly by turning the handle
North Palm Beach, FL 33408. clockwise until either the maximum stress or failure is reached.

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 D4541 − 09´1

(a)

(b)

FIG. A2.1 Photograph (a) and Schematic (b) of Type III, Self-Alignment Tester

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 D4541 − 09´1

A3. SELF-ALIGNMENT ADHESION TESTER TYPE IV (TEST METHOD D)

A3.1 Apparatus: A3.2.1 Follow the general procedures described in Sections

6 and 7. Procedures specific to Type IV testers are described in
A3.1.1 This is a self-aligning automated tester, which may
the following section.
have a self-contained pressure source and has a control module
that controls a choice of different load range detaching A3.2.2 Adhere a loading fixture to the coating based on the
assemblies, or pistons. It is shown in Fig. A3.1. epoxy manufacturers instructions, employing either a cut-off
NOTE A3.1—Precision data for Type IV instruments shown in Table 6
ring or adhesive mask to reproducibly define the area being
were obtained using the devices described in Fig. A3.1. tested. On larger sized loading fixtures, simply wipe away
excess epoxy with a cotton tipped applicator or rag.
A3.1.2 The apparatus is comprised of: (1) a loading fixture,
(2) a detaching assembly, or piston, (3) one of several control A3.2.3 Place the piston over the loading fixture and gently
modules, and (4) a pressurized air source. thread the reaction plate (top of piston) onto the loading fixture.
A3.2.4 Attach the appropriate pneumatic hoses and ensure
A3.1.3 The loading fixtures are available on many different that the control module has an air supply of at least 0.67 Mpa
sizes (3 to 75 mm) based on the particulars of the system being (100 psi) as read on the supply gauge. Zero the Piston Pressure
tested. The standard loading fixture is 12.5 mm (0.5 in) in gauge/display.
diameter. The face of the loading fixture can be rough, smooth,
A3.2.5 Ensure that the Rate Valve is closed (clockwise
curved, machined, etc.
finger tight) and then press and hold the Run button. Slowly
A3.1.4 The pistons are also available in several different open the Rate Valve (counterclockwise) and monitor the Piston
sizes, or load ranges. It is recommended that a piston is chosen Pressure gauge/display to obtain a rate of pressure increase of
so that the midpoint of the range is close to the suspected less than 1 MPa/s (100 psi/s) yet allowing for the entire test to
tensile strength of the coating to be tested. This will provide the be complete within 100 s. When the loading fixture detaches
most forgiveness in errors of assumed coating strength. from the surface or the required pressure is attained, release the
Run button.
A3.1.5 Several models of control modules are available.
The digital models may include optional accessories allowing A3.2.6 Open the Rate Valve even further (counterclock-
for features such as wireless real-time transmission of pull-tests wise) to relieve the residual pressure so the loading fixture can
via Bluetooth and your PC, LabVIEW-created software, USB be removed from the piston to prepare for the next test.
camera attachment to photo document your pulls, and com- A3.2.7 Record both the maximum pressure attained and the
puter generated reporting capabilities. specific piston used. Convert the maximum Piston Pressure to
coating tensile strength using the conversion charts or set the
A3.1.6 The pressurized air source may be (1) a self-
specific testing parameters within the software to have this step
contained miniature air cylinder for maximum portability, (2)
completed automatically.
shop (bottled) air, or (3) air from an automated pump.
A3.2.8 Photo document the test site if possible/necessary
A3.2 Procedure: using the optional USB camera.

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 D4541 − 09´1

(a)

FIG. A3.1 Photograph (a) and Schematic of Piston (b) of Type IV Self-Alignment Adhesion Tester

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 D4541 − 09´1

A4. SELF-ALIGNING ADHESION TESTER TYPE V (TEST METHOD E)

A4.1 Apparatus: cally 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
A4.1.1 This is a self-aligning tester, as shown in Fig.
required.
A4.1.11,9
NOTE A4.1—Precision data for Type V instruments shown in Table 6 A4.2 Procedure:
were obtained using the devices described as “Manual” in Fig. A4.1.
A4.2.1 Follow the general procedures described in Sections
A4.1.2 A self-aligning spherical loading fixture head is used 6 and 7. Procedures specific to Type V Testers are described in
by this tester. Load evenly distributes pulling force over the this section.
surface being tested, ensuring a perpendicular, balanced pull- A4.2.2 Ensure the pressure relief valve on the pump is
off. The diameter of the standard loading fixture 20 mm (0.78 completely open. Push the actuator handle completely down
in.) is equal to the area of the position bore in the actuator. into the actuator assembly.
Therefore, the pressure reacted by the loading fixture is the
same as the pressure in the actuator and is transmitted directly A4.2.3 Place the actuator assembly over the loading fixture
to the pressure gauge. The tester performs automatic conver- head and attach the quick coupling to the loading fixture. Close
sion calculations for the 50 mm (1.97 in.) loading fixtures and the pressure relief valve on the pump. Select the appropriate
common custom sizes 10 and 14 mm (0.39 in. and 0.55 in. loading fixture size on the display and then press the zero
respectively). button.
A4.2.4 Prime the pump by pumping the handle until the
A4.1.3 The apparatus is comprised of: a loading fixture, 10
displayed reading approaches the priming pressure as ex-
to 50 mm (0.39 and 1.97 in. respectively) diameter, hydraulic
plained in the instruction manual. Return the pump handle to
actuator by which the load is applied to the loading fixture,
its full upright position and then complete a single stroke at a
pressure gauge with LCD display, and hydraulic pump.
uniform rate of no more than 1 MPa/s (150 psi/s) as shown on
A4.1.4 The display on the pressure gauge indicates the the display until the actuator pulls the loading fixture from the
maximum force and the rate of pull. surface.
A4.1.5 The tester is available with accessories for finishes A4.2.5 Immediately following the pull, open the pressure
on plastics, metals, and wood. Special loading fixtures, typi- relief valve on the pump to release the pressure. The display
will maintain the maximum pressure reading. Record this pull
off pressure into the tester’s memory and mark the loading
fixture for future qualitative analysis.
11
The sole source of supply of the PosiTest Pull-Off Tester known to the
committee at this time is DeFelsko Corporation, 802 Proctor Avenue, Ogdensburg, A4.2.6 A version of this tester is available with an automatic
NY 13669 USA. hydraulic pump.

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 D4541 − 09´1

(a)

(b)
FIG. A4.1 Photograph (a) and Schematic (b) of Type V, Self-Aligning Tester

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 D4541 − 09´1

A5. SELF-ALIGNING ADHESION TESTER TYPE VI (TEST METHOD F)

A5.1 Apparatus: A5.2.2 Ensure that the pressure in the pull mechanism is
A5.1.1 This is a self-aligning tester, as shown in Fig. A5.1. released by opening the valve at the bottom of the cylinder.
NOTE A5.1—Precision data for Type VI instruments shown in Table 6 Turn the dragging indicator to zero in line with the gauge
were obtained using the devices described in Fig. A5.1. indicator needle.
A5.1.2 The self-aligning testing head uses four indepen- A5.2.3 Attach the self-aligning test head to the hydraulic
dently operated feet to ensure that the pull stress on the loading cable mechanism using the quick release connector on the side
fixture is evenly distributed independently of the shape of the of the test head. Return the crank handle to the start position
substrate or the angle of the loading fixture to the surface. See and ensure that the four pistons of the self-aligning head are
Fig. A5.1 level by pushing the head against a flat surface.
A5.1.3 The apparatus comprises a crank handle pull mecha-
A5.2.4 Place the relevant support ring over the loading
nism with a hydraulic cable mechanism, a self-aligning test
fixture. A support ring is not required for 25 mm, 50 mm, or 70
head rated at 6.3 kN and loading fixtures.
mm diameter loading fixtures or for 50 mm square loading
A5.1.4 A range of loading fixtures, from 2.8 to 70 mm fixtures.
diameter is available. The 20 mm diameter loading fixtures are
directly connected to the test head by means of a quick release A5.2.5 Attach the test head to the loading fixture either
connector. Other loading fixture sizes are supplied with threads directly or using the adapter, where appropriate. Close the
machined to allow connection to the self-aligning test head valve.
using an adapter. Loading fixtures with diameters in the range A5.2.6 Ensure that the hydraulic cable mechanism is not
2.8 to 5.7 mm are used with a micro self-aligning test head pulled tight. Hold the pull mechanism in one hand and operate
rated at 1 kN. the crank with the other using a smooth and regular motion to
A5.1.5 The force applied to the loading fixture is displayed ensure that the force is applied evenly until the desired value is
on a hydraulic pressure gauge with a dragging indicator that reached or the fracture occurs.
shows the maximum reading at the point where the loading
A5.2.7 Immediately following the completion of the pull,
fixture is removed from the surface. The gauge carries both PSI
open the valve to release any residual pressure and return the
and MPa values on two scales.
crank handle to the start position. The unit is now ready for the
A5.2 Procedure: next pull.
A5.2.1 Following the general procedures described in Sec- A5.2.8 Note the value indicated by the dragging indicator
tions 6 and 7, procedures specific to Type VI testers are and mark the loading fixture for further analysis as described in
described in the following section. Section 8.

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 D4541 − 09´1

(a)

(b)
FIG. A5.1 Photograph (a) and Schematic (b) of Type VI, Self-Aligning Tester

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 D4541 − 09´1

APPENDIX

(Nonmandatory Information)

X1. STRESS CALCULATION

X1.1 The stress computed in 8.2 is equal to the uniform in-situ measurement simply reflects the actual character of the
pull-off strength of the analogous rigid coating system if the applied coating system with respect to the analogous ideal rigid
applied force is distributed uniformly over the critical locus at system.
the instant of failure. For any given continuous stress distribu-
tion where the peak-to-mean stress ratio is known, the uniform X1.2 An error is introduced if the alignment of the appara-
pull-off strength may be approximated as: tus is not normal to the surface. An approximate correction by
U 5 XRo (X1.1)
the peak-to-mean stress ratio is:
R 5 R o ~ 110.14 az/d ! (X1.2)
where:
U = uniform pull-off strength, representing the greatest where:
force that could be applied to the given surface area, psi z = distance from the surface to the first gimbal or the point
(MPa), at which the force and counter force are generated by the
X = measured in situ pull-off strength calculated in 8.2, psi action of the driving mechanism, in. (mm),
(MPa), and d = diameter of the loading fixture, in. (mm),
Ro = peak-to-mean stress ratio for an aligned system. a = angle of misalignment, degrees (less than 5), and
R = maximum peak-to-mean stress ratio for the misaligned
It is important to note that a difference between these pull-off
rigid system.
strengths does not necessarily constitute an error; rather the

SUMMARY OF CHANGES

Committee D01 has identified the location of selected changes to this standard since the last issue (D4541 - 02)
that may impact the use of this standard. (Approved February 1, 2009.)

(1) The scope was modified to describe the types of substrates (3) Section 10 — The precision and bias statement was revised
covered by the test method. based on the results of a new round-robin study.
(2) Test Method A was discontinued. Test Method F and Annex (4) Editorial changes were made throughout the document.
F were added.

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