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

Adhesives Evaluated: 1. 2. 3. 4. Epoxy (72 hour recommended cure), identified as A herein Epoxy (quick set), identified as B herein Epoxy (24 hour recommended cure), identified as C herein 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 70oF 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 Tester Tester F1 H1 H2 Mean 20 1004 1261 1443 Mean of Coefficient 20 0.212 0.221 0.124 of Variation (C/v) Mean (excluding glue 13-16 855 1406 1386 failures) Mean (excluding low 17 NA 1426 NA glue failures)
Number of tests: 5 coatings x 4 adhesives

Tester P1 1357 0.099 1295 NA

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 Adhesive Adhesive Adhesive A B C 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 IOZ/E/U IOZ/A/A OZ/E/U MCUZ/ ZnM Tests MCU/MCU Number of 16 6 2 14 3 2 Failures
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 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.