Designation: D 4541 – 09

Standard Test Method for

Pull-Off Strength of Coatings Using Portable Adhesion
Testers1
This standard is issued under the fixed designation D 4541; 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.

1. Scope* accessible. Measurements are limited by the strength of adhe-

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1.1 This test method covers a procedure for evaluating the sion bonds between the loading fixture and the specimen
pull-off strength (commonly referred to as adhesion) of a surface or the cohesive strengths of the adhesive, coating
coating system from metal substrates. Pull-off strength of layers, and substrate.
coatings from concrete is described in Test Method D 7234. 1.4 This test can be destructive and spot repairs may be
The test determines either the greatest perpendicular force (in necessary.
tension) that a surface area can bear before a plug of material 1.5 The values stated in MPa (inch-pound) units are to be
is detached, or whether the surface remains intact at a pre- regarded as the standard. The values given in parentheses are
scribed force (pass/fail). Failure will occur along the weakest for information only.
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
2.1 ASTM Standards:3
and wood. Factors such as loading rate and flexibility of the substrate must
be addressed by the user/specifier. D 2651 Guide for Preparation of Metal Surfaces for Adhe-
sive Bonding
1.2 Pull-off strength measurements depend upon both ma- D 3933 Guide for Preparation of Aluminum Surfaces for
terial and instrumental parameters. Results obtained by each Structural Adhesives Bonding (Phosphoric Acid Anodiz-
test method may give different results. Results should only be ing)
assessed for each test method and not be compared with other D 3980 Practice for Interlaboratory Testing of Paint and
instruments. There are five instrument types, identified as Test Related Materials4
Methods B-F. It is imperative to identify the test method used D 7234 Test Method for Pull-Off Adhesion Strength of
when reporting results. Coatings on Concrete Using Portable Pull-Off Adhesion
NOTE 2—Method A, which appeared in previous versions of this Testers
standard, has been eliminated as its main use is for testing on concrete E 691 Practice for Conducting an Interlaboratory Study to
substrates (see Test Method D 7234). Determine the Precision of a Test Method
1.3 This test method uses a class of apparatus known as 2.2 ANSI Standard:
portable pull-off adhesion testers.2 They are capable of apply- N512 Protective Coatings (Paints) for the Nuclear Industry5
ing a concentric load and counter load to a single surface so 2.3 ISO Standard:
that coatings can be tested even though only one side is ISO 4624 Paints and Varnish—Pull-Off Test for Adhesion5

1 3
This test method is under the jurisdiction of ASTM Committee D01 on Paint For referenced ASTM standards, visit the ASTM website, www.astm.org, or
and Related Coatings, Materials, and Applications and is the direct responsibility of contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Subcommittee D01.46 on Industrial Protective Coatings. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Feb. 1, 2009. Published April 2009. Originally the ASTM website.
4
approved in 1993. Last previous edition approved in 2002 as D 4541 – 02. Withdrawn.
2 5
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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 D 4541 – 09
3. Summary of Test Method 5.1.6 Force Indicator and Calibration Information, for
3.1 The general pull-off test is performed by securing a determining the actual force delivered to the loading fixture.
loading fixture (dolly, stud) normal (perpendicular) to the 5.2 Solvent, or other means for cleaning the loading fixture
surface of the coating with an adhesive. After the adhesive is surface. Finger prints, moisture, and oxides tend to be the
cured, a testing apparatus is attached to the loading fixture and primary contaminants.
aligned to apply tension normal to the test surface. The force 5.3 Fine Sandpaper, or other means of cleaning the coating
applied to the loading fixture is then gradually increased and that will not alter its integrity by chemical or solvent attack. If
monitored until either a plug of material is detached, or a any light sanding is anticipated, choose only a very fine grade
specified value is reached. When a plug of material is detached, abrasive (400 grit or finer) that will not introduce flaws or leave
the exposed surface represents the plane of limiting strength a residue.
within the system. The nature of the failure is qualified in 5.4 Adhesive6, for securing the fixture to the coating that
accordance with the percent of adhesive and cohesive failures, does not affect the coating properties. Two component epoxies
and the actual interfaces and layers involved. The pull-off and acrylics have been found to be the most versatile.
strength is computed based on the maximum indicated load, 5.5 Magnetic or Mechanical Clamps, if needed, for holding
the instrument calibration data, and the original surface area the fixture in place while the adhesive cures.
stressed. Pull-off strength results obtained using different 5.6 Cotton Swabs, or other means for removing excess
devices may be different because the results depend on adhesive and defining the adhered area. Any method for
instrumental parameters (see Appendix X1). removing excess adhesive that damages the surface, such as
scoring (see 6.7), must generally be avoided since induced
4. Significance and Use surface flaws may cause premature failure of the coating.
5.7 Circular Hole Cutter (optional), to score through to the
4.1 The pull-off strength of a coating is an important
substrate around the loading fixture.
performance property that has been used in specifications. This
test method serves as a means for uniformly preparing and 6. Test Preparation
testing coated surfaces, and evaluating and reporting the
6.1 The method for selecting the coating sites to be prepared
results. This test method is applicable to any portable apparatus
for testing depends upon the objectives of the test and
meeting the basic requirements for determining the pull-off
agreements between the contracting parties. There are, how-
strength of a coating.
ever, a few physical restrictions imposed by the general method
4.2 Variations in results obtained using different devices or
and apparatus. The following requirements apply to all sites:
different substrates with the same coating are possible (see
6.1.1 The selected test area must be a flat surface large
Section 10). Therefore, it is recommended that the type of
enough to accommodate the specified number of replicate tests.
apparatus and the substrate be mutually agreed upon between
The surface may have any orientation with reference to
the interested parties.
gravitational pull. Each test site must be separated by at least
4.3 The purchaser or specifier shall designate a specific test
the distance needed to accommodate the detaching apparatus.
method, that is, B, C, D, E, or F when calling out this standard.
The size of a test site is essentially that of the secured loading
fixture. At least three replications are usually required in order
5. Apparatus
to statistically characterize the test area.
5.1 Adhesion Tester, commercially available, or comparable 6.1.2 The selected test areas must also have enough perpen-
apparatus specific examples of which are listed in Annex dicular and radial clearance to accommodate the apparatus, be
A1-Annex A5. flat enough to permit alignment, and be rigid enough to support
5.1.1 Loading Fixtures, having a flat surface on one end that the counter force. It should be noted that measurements close
can be adhered to the coating and a means of attachment to the to an edge may not be representative of the coating as a whole.
tester on the other end. 6.2 Since the rigidity of the substrate affects pull-off
5.1.2 Detaching Assembly (adhesion tester), having a cen- strength results and is not a controllable test variable in field
tral grip for engaging the fixture. measurements, some knowledge of the substrate thickness and
5.1.3 Base, on the detaching assembly, or an annular bearing composition should be reported for subsequent analysis or
ring if needed for uniformly pressing against the coating laboratory comparisons. For example, steel substrate of less
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surface around the fixture either directly, or by way of an than 3.2 mm (1⁄8 in.) thickness usually reduces pull-off strength
intermediate bearing ring. A means of aligning the base is results compared to 6.4 mm (1⁄4-in.) thick steel substrates.
needed so that the resultant force is normal to the surface. 6.3 Subject to the requirements of 6.1, select representative
5.1.4 Means of moving the grip away from the base in as test areas and clean the surfaces in a manner that will not affect
smooth and continuous a manner as possible so that a torsion integrity of the coating or leave a residue. To reduce the risk of
free, co-axial (opposing pull of the grip and push of the base glue failures, the surface of the coating can be lightly abraded
along the same axis) force results between them. to promote adhesion of the adhesive to the surface. If the
5.1.5 Timer, or means of limiting the loading rate to 1 MPa/s surface is abraded, care must be taken to prevent damage to the
(150 psi/s) or less for a 20 mm loading fixture so that the test
is completed in about 100 s or less. A timer is the minimum
equipment when used by the operator along with the force 6
Scotch Weld 420, available from 3M, Adhesives, Coatings and Sealers Div.,
indicator in 5.1.6. 3M Center, St. Paul, MN 55144, was used in the round robin.
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 D 4541 – 09
coating or significant loss of coating thickness. Solvent clean 7.1.2.1 Operate the instrument in accordance with Annex
the area to remove particulates after abrading. Select a solvent A1.
that does not compromise the integrity of the coating. 7.1.3 Test Method C — Self-Alignment Adhesion Tester Type
6.4 Clean the loading fixture surface as indicated by the III:
apparatus manufacturer. Failures at the fixture-adhesive inter- 7.1.3.1 Operate the instrument in accordance with Annex
face can often be avoided by treating the fixture surfaces in A2.
accordance with an appropriate ASTM standard practice for 7.1.4 Test Method D — Self-Alignment Adhesion Tester Type
preparing metal surfaces for adhesive bonding. IV:
7.1.4.1 Operate the instrument in accordance with Annex
NOTE 3—Guides D 2651 and D 3933 are typical of well-proven meth-
ods for improving adhesive bond strengths to metal surfaces.
A3.
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7.1.5 Test Method E — Self-Alignment Adhesion Tester Type

6.5 Prepare the adhesive in accordance with the adhesive V:
manufacturer’s recommendations. Apply the adhesive to the 7.1.5.1 Operate the instrument in accordance with Annex
fixture or the surface to be tested, or both, using a method A4.
recommended by the adhesive manufacturer. Be certain to 7.1.6 Test Method F— Self-Alignment Adhesion Tester Type
apply the adhesive across the entire surface. Position fixture on VI:
the surface to be tested. Carefully remove the excess adhesive 7.1.6.1 Operate the instrument in accordance with Annex
from around the fixture. (Warning—Movement, especially A5.
twisting, can cause tiny bubbles to coalesce into large holidays 7.2 Select an adhesion-tester with a detaching assembly
that constitute stress discontinuities during testing.) having a force calibration spanning the range of expected
NOTE 4—Adding about 1 percent of #5 glass beads to the adhesive values along with its compatible loading fixture. Mid-range
assists in even alignment of the test fixture to the surface. measurements are usually the best, but read the manufacturer’s
operating instructions before proceeding.
6.6 Based on the adhesive manufacturer’s recommendations 7.3 If a bearing ring or comparable device (5.1.3) is to be
and the anticipated environmental conditions, allow enough used, place it concentrically around the loading fixture on the
time for the adhesive to set up and reach the recommended coating surface. If shims are required when a bearing ring is
cure. During the adhesive set and early cure stage, a constant employed, place them between the tester base and bearing ring
contact pressure should be maintained on the fixture. Magnetic rather than on the coating surface.
or mechanical clamping systems work well, but systems 7.4 Carefully connect the central grip of the detaching
relying on tack, such as masking tape, should be used with care assembly to the loading fixture without bumping, bending, or
to ensure that they do not relax with time and allow air to otherwise prestressing the sample and connect the detaching
intrude between the fixture and the test area. assembly to its control mechanism, if necessary. For nonhori-
6.7 Scoring around the fixture violates the fundamental in zontal surfaces, support the detaching assembly so that its
situ test criterion that an unaltered coating be tested. If scoring weight does not contribute to the force exerted in the test.
around the test surface is employed, extreme care is required to 7.5 Align the device according to the manufacturer’s in-
prevent micro-cracking in the coating, since such cracks may structions and set the force indicator to zero.
cause reduced adhesion values. Scored samples constitute a
different test, and this procedure should be clearly reported NOTE 6—Proper alignment is critical, see Appendix X1. If alignment is
required, use the procedure recommended by the manufacturer of the
with the results. Scoring is only recommended for thicker-film
adhesion tester and report the procedure used.
coatings, that is, thicknesses greater than 500 µm (20 mils),
reinforced coatings and elastomeric coatings. Scoring, if per- 7.6 Increase the load to the fixture in as smooth and
formed, shall be done in a manner that ensures the cut is made continuous a manner as possible, at a rate of 1 MPa/s (150
normal to the coating surface and in a manner that does not psi/s) or less for a 20 mm loading fixture so that the test is
twist or torque the test area and minimizes heat generated and completed in about 100 s or less.
edge damage or microcracks to the coating and the substrate. 7.7 Record the force attained at failure or the maximum
For thick coatings it is recommended to cool the coating and force applied.
substrate during the cutting process with water lubrication. 7.8 If a plug of material is detached, label and store the
fixture for qualification of the failed surface in accordance with
NOTE 5—A template made from plywood with a hole of the same size 8.3.
drilled through it has been found to be an effective method to limit
sideways movement of the drill bit.
7.9 Report any departures from the procedure such as
possible misalignment, hesitations in the force application, etc.
6.8 Note the approximate temperature and relative humidity
during the time of test. 8. Calculation and Interpretation of Results
8.1 If instructed by the manufacturer, use the instrument
7. Test Procedure calibration factors to convert the indicated force for each test
7.1 Test Methods: into the actual force applied.
7.1.1 Test Method A (discontinued). 8.2 Either use the calibration chart supplied by the manu-
7.1.2 Test Method B — Fixed Alignment Adhesion Tester facturer or compute the relative stress applied to each coating
Type II: sample as follows:

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 D 4541 – 09
X 5 4F/pd2 (1) 9.1.4 Description of the test system, if possible, by the
indexing scheme outlined in 8.3 including: product identity and
where: generic type for each coat and any other information supplied,
X = greatest mean pull-off stress applied during a pass/fail the substrate identity (thickness, type, orientation, etc.), and the
test, or the pull-off strength achieved at failure. Both adhesive used.
have units of MPa (psi), 9.1.5 Test results.
F = actual force applied to the test surface as determined in 9.1.5.1 Date, test location, testing agent.
8.1, and 9.1.5.2 For pass/fail tests, stress applied along with the
d = equivalent diameter of the original surface area
result, for example, pass or fail and note the plane of any
stressed having units of inches (or millimetres). This is
failure (see 8.3 and ANSI N512).
usually equal to the diameter of the loading fixture.
9.1.5.3 For tests to failure, report all values computed in 8.2
8.3 For all tests to failure, estimate the percent of adhesive
along with the nature and location of the failures as specified in
and cohesive failures in accordance to their respective areas
8.3, or, if only the average strength is required, report the
and location within the test system comprised of coating and
average strength along with the statistics.
adhesive layers. A convenient scheme that describes the total
9.1.5.4 If corrections of the results have been made, or if
test system is outlined in 8.3.1 through 8.3.3. (See ISO 4624.)
certain values have been omitted such as the lowest or highest
NOTE 7—A laboratory tensile testing machine is used in ISO 4624. values or others, reasons for the adjustments and criteria used.
8.3.1 Describe the specimen as substrate A, upon which 9.1.5.5 For any test where scoring was employed, indicate it
successive coating layers B, C, D, etc., have been applied, by placing a footnote superscript beside each data point
including the adhesive, Y, that secures the fixture, Z, to the top affected and a footnote to that effect at the bottom of each page
coat. on which such data appears. Note any other deviations from the
8.3.2 Designate cohesive failures by the layers within which procedure.
they occur as A, B, C, etc., and the percent of each.
8.3.3 Designate adhesive failures by the interfaces at which 10. Precision and Bias 7,8
they occur as A/B, B/C, C/D, etc., and the percent of each. 10.1 The precision of this test method is based on an
8.4 A result that is very different from most of the results interlaboratory study of Test Method D 4541 conducted in
may be caused by a mistake in recording or calculating. If 2006. Analysts from seven laboratories tested six different
either of these is not the cause, then examine the experimental coatings applied to 1⁄4 in. thick hot-rolled carbon steel plates
circumstances surrounding this run. If an irregular result can be using five different adhesion testers. Every “test result” repre-
attributed to an experimental cause, drop this result from the sents an individual determination. In order to standardize and
analysis. However, do not discard a result unless there are valid balance the data, any pull which exceeded the tester’s upper
nonstatistical reasons for doing so or unless the result is a limit with the available accessories at the time of testing was
statistical outlier. Valid nonstatistical reasons for dropping eliminated from the statistical analysis. Any pull in which there
results include alignment of the apparatus that is not normal to was 50 % or more glue failure was also eliminated from the
the surface, poor definition of the area stressed due to improper statistical analysis. If four valid pulls were obtained from one
application of the adhesive, poorly defined glue lines and operator for a given material, the fourth was eliminated and the
boundaries, holidays in the adhesive caused by voids or first three valid replicate test results (from one operator) for
inclusions, improperly prepared surfaces, and sliding or twist- each material were included in the statistical analysis. Practice
ing the fixture during the initial cure. Scratched or scored E 691 was followed for the design and analysis of the data; the
samples may contain stress concentrations leading to prema- details are given in Research Report No. D01–1147.
ture fractures. Dixon’s test, as described in Practice D 3980,
NOTE 8—The pull-off strength of two of the coatings, identified during
may be used to detect outliers. the round robin as Coating A and Coating F, exceeded the measurement
8.5 Disregard any test where glue failure represents more limits of the testers with the accessories available at the time of testing,
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than 50 % of the area. If a pass/fail criterium is being used and and were therefore eliminated from the statistical analysis.
a glue failure occurs at a pull-off strength greater than the 10.1.1 Repeatability—Two test results obtained within one
criterium, report the result as “pass with a pull-off strength > laboratory shall be judged not equivalent if they differ by more
{value obtained}...” than the “r” value for that material; “r” is the interval
8.6 Further information relative to the interpretation of the representing the critical difference between two test results for
test results is given in Appendix X1. the same material, obtained by the same operator using the
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9. Report same equipment on the same day in the same laboratory.

9.1 Report the following information: 10.1.1.1 Repeatability limits are listed in Tables 1-5.
9.1.1 Brief description of the general nature of the test, such 10.1.2 Reproducibility—Two test results shall be judged not
as, field or laboratory testing, generic type of coating, etc. equivalent if they differ by more than the “R” value for that
9.1.2 Temperature and relative humidity and any other
pertinent environmental conditions during the test period. 7
Supporting data are available from ASTM International Headquarters. Request
9.1.3 Description of the apparatus used, including: appara- RR: D01-1094.
tus manufacturer and model number, loading fixture type and 8
Supporting data have been filed at ASTM International Headquarters and may
dimensions, and bearing ring type and dimensions. be obtained by requesting Research Report RR: D01–1147.

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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
x sr sR r R x 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
x r % of average R % of average x 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
x sr sR r R x 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
x r % of average R % of average x 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) 10.1.3 Any judgment in accordance with these two state-
Repeatability Reproducibility ments would have an approximate 95 % probability of being
Repeatability Reproducibility
Coating Average Standard Standard
Limit Limit
correct.
Deviation Deviation
10.2 Bias—At the time of the study, there was no accepted
x sr sR r SR
reference material suitable for determining the bias for this test
B 2458 146 270 408 755
C 1232 31 116 87 324
method, therefore no statement is being made.
D 2707 155 233 434 651 10.3 The precision statement was determined through sta-
E 2354 163 273 456 764 tistical examination of 394 results, produced by analysts from
Coating Average
Repeatability Reproducibility seven laboratories, on four coatings, using five different
Limit Limit
instruments. Different coatings were used as a means to
x r % of average R % of average
achieve a range of pull-off strengths covering the operating
B 2458 408 16.6 755 30.7
range of all the instruments.
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C 1232 87 7.1 324 26.3

D 2707 434 16.0 651 24.0 10.3.1 Results obtained by the same operator using instru-
E 2354 456 19.4 764 32.5 ments from the same Method should be considered suspect if
Avg. 14.8 28.4 they differ in percent relative by more than the Intralaboratory
values given in Table 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
material; “R” is the interval representing the difference be- than the Interlaboratory values given in Table 6.
tween two test results for the same material, obtained by
different operators using different equipment in different labo- 11. Keywords
ratories. 11.1 adhesion; coatings; field; metal substrates; paint; por-
10.1.2.1 Reproducibility limits are listed in Tables 1-5. table; pull-off strength; tensile test

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D 4541 – 09
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. A1.1.9,10 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 A1.2.2 Align or shim the three instrument swivel pads of the
were obtained using the devices described ed in Fig. A1.1.
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 A1.2.3 Take up the slack between the various members and
circular T-bolt head on the other end, a central grip for slide the dragging (force) indicator located on the tester to zero.
engaging the loading fixture that is forced away from a tripod A1.2.4 Firmly hold the instrument with one hand. Do not
base by the interaction of a hand wheel (or nut), and a coaxial allow the base to move or slide during the test. With the other
bolt connected through a series of belleville washers, or springs hand, turn the hand wheel clockwise using as smooth and
in later models, that acts as both a torsion relief and a spring constant motion as possible. Do not jerk or exceed a stress rate
that displaces a dragging indicator with respect to a 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
A1.1.4 The devices are available in four ranges: From 3.5, will not be removed by a shearing force or misalignment, thus
7.0, 14, and 28 MPa (0 to 500, 0 to 1000, 0 to 2000, and 0 to negating the results. The maximum stress must be reached
4000 psi). within about 100 s.
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
9
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.
10
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, 1which you may attend the bottom of the dragging indicator.
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(a)

(b)

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

Copyright ASTM International 7

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 D 4541 – 09

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

A2.1 Apparatus: A2.1.5 The testers are available in three standard working
A2.1.1 This is a self-aligning tester, as shown in Fig. ranges: 0 to 10 MPa (0 to 1500 psi), 0 to 15 MPa (0 to 2250
A2.1.11,10 psi), 0 to 20 MPa (0 to 3000 psi). Special loading fixtures
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
A2.1.4 The force is indicated by the maximum hydraulic from the loading fixture. Decrease pressure to zero and remove
pressure as displayed on the gauge, since the effective areas of the test loading fixture.
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
11 the surface to be tested and that the hose is straight.
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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 D 4541 – 09

(a)
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(b)

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

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 D 4541 – 09

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

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

A3.1.1 This is a self-aligning automated tester, which may 6 and 7. Procedures specific to Type IV testers are described in
have a self-contained pressure source and has a control module the following section.
that controls a choice of different load range detaching assem- A3.2.2 Adhere a loading fixture to the coating based on the
blies, or pistons. It is shown in Fig. A3.1. epoxy manufacturers instructions, employing either a cut-off
ring or adhesive mask to reproducibly define the area being
NOTE A3.1—Precision data for Type IV instruments shown in Table 6 tested. On larger sized loading fixtures, simply wipe away
were obtained using the devices described in Fig. A3.1. excess epoxy with a cotton tipped applicator or rag.
A3.1.2 The apparatus is comprised of: (1) a loading fixture, A3.2.3 Place the piston over the loading fixture and gently
(2) a detaching assembly, or piston, (3) one of several control thread the reaction plate (top of piston) onto the loading fixture.
modules, and (4) a pressurized air source. 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
A3.1.5 Several models of control modules are available. Run button.
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
A3.1.6 The pressurized air source may be (1) a self- coating tensile strength using the conversion charts or set the
contained miniature air cylinder for maximum portability, (2) specific testing parameters within the software to have this step
shop (bottled) air, or (3) air from an automated pump. completed automatically.
A3.2.8 Photo document the test site if possible/necessary
A3.2 Procedure: using the optional USB camera.

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 D 4541 – 09

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(a)

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

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 D 4541 – 09

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
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A4.1.1 This is a self-aligning tester, as shown in Fig. use on curved surfaces and when higher pull-off pressures are
A4.1.12,10 required.
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 A4.2.3 Place the actuator assembly over the loading fixture
same as the pressure in the actuator and is transmitted directly head and attach the quick coupling to the loading fixture. Close
to the pressure gauge. The tester performs automatic conver- the pressure relief valve on the pump. Select the appropriate
sion calculations for the 50 mm (1.97 in.) loading fixtures and loading fixture size on the display and then press the zero
common custom sizes 10 and 14 mm (0.39 in. and 0.55 in. button.
respectively). 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
12 fixture for future qualitative analysis.
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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(a)

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

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 D 4541 – 09

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.
Turn the dragging indicator to zero in line with the gauge
NOTE A5.1—Precision data for Type VI instruments shown in Table 6
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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D 4541 – 09
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(a)

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

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 D 4541 – 09

APPENDIX

(Nonmandatory Information)

X1. STRESS CALCULATION

X1.1 The stress computed in 8.2 is equal to the uniform X1.2 An error is introduced if the alignment of the
pull-off strength of the analogous rigid coating system if the apparatus is not normal to the surface. An approximate
applied force is distributed uniformly over the critical locus at correction by the peak-to-mean stress ratio is:
the instant of failure. For any given continuous stress distribu- R 5 Ro ~1 1 0.14 az/d! (X1.2)
tion where the peak-to-mean stress ratio is known, the uniform
pull-off strength may be approximated as: where:
U 5 XRo (X1.1) z = distance from the surface to the first gimbal or the point
at which the force and counter force are generated by
the action of the driving mechanism, in. (mm),
where: d = diameter of the loading fixture, in. (mm),
U = uniform pull-off strength, representing the greatest a = angle of misalignment, degrees (less than 5), and
force that could be applied to the given surface area, R = maximum peak-to-mean stress ratio for the misaligned
psi (MPa), rigid system.
X = measured in situ pull-off strength calculated in 8.2,
psi (MPa), and
Ro = peak-to-mean stress ratio for an aligned system.
It is important to note that a difference between these pull-off
strengths does not necessarily constitute an error; rather the
in-situ measurement simply reflects the actual character of the
applied coating system with respect to the analogous ideal rigid
system.

SUMMARY OF CHANGES

Committee D01 has identified the location of selected changes to this standard since the last issue
(D 4541 - 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 (4) Editorial changes were made throughout the document.
Annex F were added.

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