The following column was excerpted from a research paper presented at the SSPC 2001

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






Coating Systems Evaluated:

1. Inorganic zinc primer / polyamide epoxy intermediate / acrylic polyurethane topcoat
(IOZ/E/U)
2. Inorganic zinc primer / acrylic latex intermediate / acrylic latex topcoat (IOZ/A/A)
3. Organic (epoxy) zinc primer / polyamide epoxy intermediate / acrylic polyurethane
topcoat (OZ/E/U)
4. Moisture cure urethane zinc primer / moisture cure urethane intermediate /
moisture cure urethane topcoat (MCUZ/MCU/MCU)
5. 100% Zinc metallizing using electric arc application (ZnM)

Adhesion Testers Employed:

1. Fixed-alignment tester (ASTM D4541, Annex A2) identified as F1 herein
2. Self-aligning tester (ASTM D4541, Annex A3) Hydraulic, identified as H1 herein
3. Self-aligning tester (ASTM D4541, Annex A5) Hydraulic, identified as H2 herein
4. Self-aligning tester (ASTM D4541, Annex A4) Pneumatic, identified as P1 herein

Adhesives Evaluated:

1. Epoxy (72 hour recommended cure), identified as A herein
2. Epoxy (quick set), identified as B herein
3. Epoxy (24 hour recommended cure), identified as C herein
4. Cyanoacrylate Gel, identified as D herein

Adhesives Cure Times Evaluated:

1. 4 hours
2. 16 hours
3. 72 hours



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 70
o
F and 50% relative
humidity. Varying conditions (e.g., lower temperature) may require additional adhesive
cure time.




Variability in Adhesion Data Among
Adhesion Test Devices (16 Hour Adhesive Cure Time)

Tables 1-5 depict the range in adhesion data on the same coating system using
four different test devices (average of three adhesion pulls for each tester). The data are
presented for four adhesives, on each of five coating systems, and are based on averaged
test results. All data is based on a nominal 16 hour adhesive cure time and represents a
combination of both coating breaks and glue failures.

Table 1 Variability in Adhesion Data
Among Test Devices and Adhesive Type IOZ/E/U
Adhesive Type Tensile Adhesion Range - Four Testers
Epoxy 1 (rec. 72 hr. cure) 1133 1527 psi
Epoxy 2 (quick set) 333 1753 psi
Epoxy 3 (rec. 24 hr. cure) 1500 1888 psi
Cyanoacrylate Gel 1293 1767 psi

Table 2 Variability in Adhesion Data
Among Test Devices and Adhesive Type IOZ/A/A
Adhesive Type Tensile Adhesion Range - Four Testers
Epoxy 1 (rec. 72 hr. cure) 767 1556 psi
Epoxy 2 (quick set) 533 1713 psi
Epoxy 3 (rec. 24 hr. cure) 867 2333 psi
Cyanoacrylate Gel 967 1481 psi

Table 3 Variability in Adhesion Data
Among Test Devices and Adhesive Type OZ/E/U
Adhesive Type Tensile Adhesion Range - Four Testers
Epoxy 1 (rec. 72 hr. cure) 1000 2173 psi
Epoxy 2 (quick set) 1133 1550 psi
Epoxy 3 (rec. 24 hr. cure) 1567 2227 psi
Cyanoacrylate Gel 800 2083 psi

Table 4 Variability in Adhesion Data
Among Test Devices and Adhesive Type MCUZ/MCU/MCU
Adhesive Type Tensile Adhesion Range - Four Testers
Epoxy 1 (rec. 72 hr. cure) 517 1583 psi
Epoxy 2 (quick set) 800 1481 psi
Epoxy 3 (rec. 24 hr. cure) 1275 1600 psi
Cyanoacrylate Gel 700 1283 psi







Table 5 Variability in Adhesion Data
Among Test Devices and Adhesive Type ZnM
Adhesive Type Tensile Adhesion Range - Four Testers
Epoxy 1 (rec. 72 hr. cure) 383 970 psi
Epoxy 2 (quick set) 443 840 psi
Epoxy 3 (rec. 24 hr. cure) 517 1233 psi
Cyanoacrylate Gel 417 917 psi

Variability in Adhesion Data Between Four
Different Adhesives (16 Hour Adhesive Cure Time)

Tables 6-10 depict the range in adhesion data on the same coating system using
four different adhesives. The data are presented for four test devices, on each of five
coating systems, and are based on averaged test results (average of three adhesion pulls
for each tester). All data is based on a nominal 16 hour adhesive cure time, and represents
a combination of both coating breaks and glue failures.

Table 6 Variability in Adhesion Data
Among Adhesive Types IOZ/E/U
Tester Type Tensile Adhesion Range Four Adhesives
Fixed Alignment (F1) 1133 1767 psi
Hydraulic 1 (H1) 333 1500 psi
Hydraulic 2 (H2) 1293 1820 psi
Pneumatic (P2) 1454 1888 psi

Table 7 Variability in Adhesion Data
Among Adhesive Types IOZ/A/A
Tester Type Tensile Adhesion Range Four Adhesives
Fixed Alignment (F1) 767 967 psi
Hydraulic 1 (H1) 533 2333 psi
Hydraulic 2 (H2) 1327 1713 psi
Pneumatic (P2) 1461 1576 psi

Table 8 Variability in Adhesion Data
Among Adhesive Types OZ/E/U
Tester Type Tensile Adhesion Range Four Adhesives
Fixed Alignment (F1) 800 - 1700 psi
Hydraulic 1 (H1) 1133 2083 psi
Hydraulic 2 (H2) 1493 2227 psi
Pneumatic (P2) 1290 1909 psi








Table 9 Variability in Adhesion Data
Among Adhesive Types MCUZ/MCU/MCU
Tester Type Tensile Adhesion Range Four Adhesives
Fixed Alignment (F1) 517 - 1275 psi
Hydraulic 1 (H1) 800 1600 psi
Hydraulic 2 (H2) 1220 1463 psi
Pneumatic (P2) 1019 1481 psi

Table 10 Variability in Adhesion Data
Among Adhesive Types ZnM
Tester Type Tensile Adhesion Range Four Adhesives
Fixed Alignment (F1) 383 517 psi
Hydraulic 1 (H1) 443 1233 psi
Hydraulic 2 (H2) 780 987 psi
Pneumatic (P2) 624 957 psi

STATISTICAL TRENDS

The data below includes a comparison of the adhesion testers (Table ST1), a
comparison of the number of glue failures based on the adhesive (Table ST2), the coating
(ST3) and adhesion tester (ST4), a comparison between the five coating systems (Table
ST5), and a comparison of the adhesives employed (Table ST6).

Table ST1 - Comparison of Adhesion Testers (values in psi)
Statistic No. of Tests Tester
F1
Tester
H1
Tester
H2
Tester
P1
Mean 20 1004 1261 1443 1357
Mean of Coefficient
of Variation (C/v)
20 0.212 0.221 0.124 0.099
Mean (excluding glue
failures)
13-16 855 1406 1386 1295
Mean (excluding low
glue failures)
17 NA 1426 NA NA
Number of tests: 5 coatings x 4 adhesives

Based on this data, there is a statistically significant difference (at a 95%
confidence level) between the mean values generated using the fixed alignment and the
three other test devices (hydraulic tester 1, hydraulic tester 2 and the pneumatic tester).
However, the differences within the latter group are not statistically significant. Further,
the mean of the coefficient of variation (mean C/v) is higher for the fixed alignment and
hydraulic tester 1, compared to both the pneumatic tester and hydraulic tester 2, which
have a lower mean C/v. The mean trend is slightly altered when glue failures are
eliminated from the data set.





Table ST2 - Comparison of Number of Adhesive (glue) Failures (by adhesive)
Statistic No. of Tests Adhesive
A
Adhesive
B
Adhesive
C
Adhesive
D
Number of Failures 20 4 12 2 7
Number of tests: 5 coatings x 4 testers

Adhesive B generated the highest number of adhesive (glue) failures. This
adhesive is marketed as a quick set product. Adhesives A and C are footnoted in
ASTM D4541 as suitable for use. These adhesives generated the lowest number of glue
failures.

Table ST3 - Comparison of Number of Adhesive (glue) Failures (by coating system)
Statistic No. of
Tests
IOZ/E/U IOZ/A/A OZ/E/U MCUZ/
MCU/MCU
ZnM
Number of
Failures
16 6 2 14 3 2
Number of tests: 4 adhesives x 4 testers

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
A
Adhesive
B
Adhesive
C
Adhesive
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
Tests
IOZ/E/U IOZ/A/A OZ/E/U MCUZ/
MCU/MCU
ZnM
Mean 16 1471 1333 1557 1222 749
Mean of
Coefficient of
Variation (C/v)
16 0.108 0.177 0.185 0.178 0.219
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
A
Adhesive
B
Adhesive
C
Adhesive
D
Mean 20 1199 1146 1504 1217
Mean of Coefficient
of Variation (C/v)
20 0.151 0.184 0.140 0.219
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.