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PAPER Tensile - Adhesion ASTM D4541
PAPER Tensile - Adhesion ASTM D4541
Conference and Exhibition. A complete copy of the research paper and the data tables
and graphs is published in the 2001 SSPC Conference Proceedings.
TENSILE ADHESION:
SPECIFYING THE TEST? SPECIFY THE TEST INSTRUMENT!
William D. Corbett
Technical Services Manager
KTA-Tator, Inc.
INTRODUCTION
The adhesion of the coating system shall be measured in accordance with
ASTM D4541. The adhesion shall be a minimum of 400 psi. What seems like a
straightforward specification requirement can lead to controversy at the time of
enforcement. Because many specifications do not specify the type of adhesion tester to
use, the minimum adhesion requirement becomes variable. For example, if the contractor
uses adhesion tester A and does not achieve the minimum adhesion value, then chooses
adhesion tester B and meets the minimum adhesion requirements of the specification,
does the coating pass? The answer is almost certainly yes, unless the specifier specifies
the test instrument to be used.
Tensile (pull-off) adhesion testing (ASTM D 4541) is becoming a more widely
specified testing requirement for shop- and field-applied liquid coatings, and is a
common quality control specification requirement during the application of metallizing.
Coating manufacturers use this procedure during formulation testing of new coatings and
publish tensile adhesion values on technical data bulletins, and the National
Transportation Product Evaluation Program (NTPEP; AASHTO Specification R31)
coating system qualification program references tensile adhesion testing as a testing
criterion.
The most recent version of ASTM D 4541 (2004) references five adhesion testers
(Annex A1-A5), two of which are fixed alignment and three are self-aligning. Data
published in Appendix X1 reveals different pull-off strengths on four test specimens
when using the various adhesion testers, based on an interlaboratory round-robin study
conducted by ASTM several years ago. Therefore, when different testers are employed, it
is difficult for specifiers to compare the tensile adhesion characteristics within a given
generic coating system category, or to compare the adhesion quality of different coating
systems.
The researcg paper presented at SSPC in 2001 explored the relative differences in
adhesion values generated between four adhesion referenced in ASTM D4541
(mechanical, hydraulic and pneumatic). The study involved four generic liquid-applied
industrial coating systems and one electric arc-applied zinc metallizing, all on steel.
Further, the effects of various adhesives and curing times were investigated.
BACKGROUND
The ASTM testing procedure provides a method for evaluating the pull-off
strength (adhesion) of a coating by applying the maximum perpendicular force that the
coated surface can withstand until the weakest plane causes a break to occur within the
coating system or causes the loading fixture to become detached. The tensile value is
stated in pounds per square inch (psi), kilopascals (KPa), or megapascals (MPa). The
break is defined according to the weakest plane, and is identified as either an adhesion,
cohesion or adhesive (glue) break.
The testing procedure employs pull-off adhesion testers that are capable of
applying a simultaneous concentric and counter load to the surface, even though only one
side of the surface is accessible. A loading fixture (e.g., pull stub or dolly) is secured to
the coated surface using an adhesive. The contact surface of the loading fixture is cleaned
and sometimes abraded prior to application of the adhesive to enhance the bond of the
adhesive to the loading fixture. Additionally, the coated surface can also be gently
cleaned using a fine grit paper (e.g., 400) to enhance the adhesion of the adhesive to the
coated surface (this is particularly important when tests are conducted on glossy
coatings). Care must be taken however to avoid introducing flaws in the surface of the
coating which could cause a reduction in adhesion strength. In the past, it was common
practice by some to score the coating around the perimeter of the pull stub. However,
scoring the coating is not recommended by the standard as it may cause microcracking of
the coating and generate lower adhesion values. After the adhesive cures, a test apparatus
is attached to the loading fixture and the perpendicular force is gradually increased until a
break occurs, or the maximum adhesion value is obtained without generating a break. If a
break occurs, the maximum load value and the location of the break are recorded.
EXPERIMENTAL DESIGN
Because of the apparent variability in tensile adhesion results reported in ASTM
D4541a research initiative was undertaken to explore the relative differences in adhesion
values based on the testing of five (5) industrial coating systems (listed below). The
research was also conducted to determine if the adhesive used to attach the loading
fixture to the coated substrate and the cure time of the adhesive itself have an impact on
the adhesion data. The research included four (4) adhesives and three (3) adhesive curing
times for each of four (4) adhesion testers.
Substrate: Commercial Grade Hot Rolled Carbon Steel
Surface Preparation:
1. Liquid-applied coatings: Near White Metal Blast (SSPC-SP10), 2-3 mil surface profile
2. Metallizing: White Metal Blast (SSPC-SP5), 3-4 mil surface profile
Adhesives Evaluated:
1.
2.
3.
4.
RESEARCH RESULTS
Adhesives were cured for 4 hours, 16 hours and 72 hours, independent of the
adhesive manufacturers recommended cure time. The four hour cure time resulted in a
large number of glue failures (primarily for the epoxy adhesives). There also did not
appear to be any real advantage to allowing the adhesive cure for more than 16 hours
prior to testing (i.e., 72 hours). Therefore, the statistical trends from the research are
based on the 16 hour adhesive cure variable. A minimum overnight adhesive cure is also
a reasonable time frame for conducting this type of testing. It should be recognized that
the 16 hour cure was based on a nominal air temperature of 70oF and 50% relative
humidity. Varying conditions (e.g., lower temperature) may require additional adhesive
cure time.
Tester
P1
1357
0.099
1295
NA
The coating systems containing the polyurethane topcoat generated the highest
number of adhesive (glue) failures. The product was high gloss, with a smooth, slick
surface. This data reinforces the need to lightly scarify the surface of the coating using
fine sandpaper (e.g., 400 grit or finer, as prescribed in the ASTM standard), in order to
enhance the adhesion of the glue to the coated surface. While ASTM cautions the user
about the possibility of introducing flaws in the coating, this procedure may be necessary
in order to avoid glue failures. Alternatively, the user could attach twice the number of
pull stubs (e.g., 6) with the hope that three of the six would generate acceptable values
without glue failures.
Table ST4 - Comparison of Number of Adhesive (glue) Failures (by tester)
Statistic
No. of Tests Adhesive Adhesive Adhesive Adhesive
A
B
C
D
Number of Failures
20
6
7
7
5
Number of tests: 5 coatings x 4 testers
Based on the data in Table ST4, it does not appear that one particular tester is
more susceptible to generating a greater number glue failures than another tester.
Table ST5 - Comparison of Adhesion Data (by coating system; values in psi)
Statistic
No. of IOZ/E/U IOZ/A/A OZ/E/U
MCUZ/
ZnM
Tests
MCU/MCU
Mean
16
1471
1333
1557
1222
749
Mean of
16
0.108
0.177
0.185
0.178
0.219
Coefficient of
Variation (C/v)
Number of tests: 4 adhesives x 4 testers
The data presented in Table ST5 is for reference only. No conclusions can be
drawn, since comparisons across coating systems will not generate any useful data
relating to the goals of this research effort.
Table ST6 - Comparison of Adhesion Data (by adhesive type; values in psi)
Statistic
No. of Tests Adhesive Adhesive Adhesive Adhesive
A
B
C
D
Mean
20
1199
1146
1504
1217
Mean of Coefficient
20
0.151
0.184
0.140
0.219
of Variation (C/v)
Number of tests: 5 coatings x 4 testers
Based on the data in Table ST6, Adhesive C generated the highest mean tensile
adhesion data and the lowest mean coefficient of variation. This result is statistically
significant at a 95% confidence level. Adhesive C is footnoted in ASTM D4541 as
suitable for use. However, Adhesive C manufacturer recommends a minimum cure
time of 24 hours.
CONCLUSIONS
Based on the data generated by this research initiative, it is apparent that there are
several variables that can influence tensile (pull-off) adhesion test data. These variables
include the type of adhesive that is used to attach the loading fixture (pull stub), the
period of time the adhesive is permitted to cure before initiating tensile forces, and the
test device that is ultimately chosen to perform the testing.
Based on this limited data set, it appears that the precision of the data generated
by the pneumatic adhesion tester (ASTM D4541, Appendix A4) and the hydraulic
adhesion tester Appendix A5) are better than the precision of the data for the fixed
alignment tester (ASTM D4541, Appendix A2) and the other version of a hydraulic tester
(ASTM D4541, Appendix A3). It also appears that Adhesive C generates the highest
adhesion values (of the coating systems tested) and the least number of glue breaks,
based on the 16 hour adhesive cure time data.
Specifications should specifically state the type of adhesion tester that is to be
used and perhaps the type of adhesive to employ when conducting this type of testing.
The specification should also clarify whether the specified minimum adhesion value is
the average of at least three tests (as suggested by ASTM D4541) or the minimum value
of any single test.
Facility owners are cautioned when comparing the performance characteristics
(specifically tensile adhesion) of a generic category of coating from various
manufacturers to ensure that the test data reported in the technical data bulletins were
generated using the same test device, and if possible the same adhesive and adhesive cure
time.