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Never AgAiN

AdhesioN TesT MeThods MAkiNg sure The resulTs sTick

By Mike OBrien

dhesion testing is commonly used during coating failure investigations; however, sometimes the wrong type of adhesion test is performed, the results are misinterpreted, or the procedures and reporting requirements in the test methods are disregarded. This article addresses some common issues related to ASTM D4541 and ASTM D6677 adhesion testing and provides readers with a proper understanding of differences between these two test methods.

Different ADhesiOn tests Different results

Several years ago, a consultant, working for a large inspection firm in the United

States, conv inced state Depar tment of Tr a nspor t at ion (DOT) personnel that the adhesion of an inorganic zinc (IOZ) primer was inadequate on a large bridge with over 400,000 square feet (37,161.22m 2) of steel. The consultant recommended that all coatings be removed and replaced on this the bridge. This recommendation was based primarily on qualitative and subjective testing he conducted on portions of the bridge, reportedly in accordance with ASTM D6677. According to the consultants report, greater than 61% of ASTM D6677 adhesion tests conducted on the exterior, and 65% of the tests on the interior box girders displayed poor cohesion strength

Above ASTM D4541 (Test Method E) showing 65% cohesive failure in IOZ primer, 20% glue failure, and 15% cohesive failure in red topcoat.

The purpose of the procedures within a standard is to ensure that different individuals perform the test following the same procedures and that they report the results using the same criteria.

of the inorganic zinc. However, the consultant did not follow the procedures contained within ASTM D6677 and even developed his own rating system, disregarding the rating system contained within the standard. Two other consultants, one hired by the general contractor and the other hired by t he fabricator, per formed adhesion tests using ASTM D4541, (a quantitative adhesion test method), and their results provided a completely different picture regarding the adhesion of the coating system. ASTM D4541 testing indicated that approximately 96% of the areas tested displayed satisfactory adhesion. Why such different results? These two test methods differ significantly in several ways. One test is quantitative, and the other is qualitative and subjective. ASTM D6677 states that the test method is subjective and qualitative and does not have any known correlation to

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other test methods (pull-off, tape, etc). Additionally, it states, Other adhesion test methods may be useful in obtaining quantitative results (See D2197, D3359, D4541, and D7234). Regardless of the explicit statements contained within ASTM D6677, the DOTs consultant refused to accept the results of more than 260 adhesion tests performed by two other consultants in accordance with ASTM D4541. As a result of the DOTs consultants allegation that the coating system would likely fail catastrophically if not removed, the steel fabricator and the general contractor each spent a substantial sum of money on consultants and legal fees.

Overview Of AstM D4541 & AstM D6677

There are several ASTM test methods for assessing the adhesion of liquid-applied coatings to a substrate or to a previously applied coating. These test methods are as follows: (1) ASTM D3359, Standard Method for Measuring Adhesion by Tape Test, (2) ASTM D4541, Standard Test Method for Pull Off Strength of Coat i ngs Usi ng Por table Ad hesion Testers, and (3) ASTM D6677, Standard Test Method for Evaluating Adhesion by Knife. (Note: ASTM D7234, Standard Test Method for Pull Off Adhesion Strength of Coatings on Concrete Using Portable Pull Off Adhesion Testers, addresses adhesion testing of coatings on a concrete substrate.) This article only discusses ASTM D4541 and ASTM D6677. The reader is advised to obtain a copy of each standard and to follow it when performing testing.

AstM D4541
This quantitative test method involves a procedure for evaluating the pull-off strength of a coating system from metal substrates using portable mechanical, hydraulic, or pneumatic adhesion testers. It ma ximizes tensile stress. Failure occurs at the weakest plane within the system, which includes the substrate, each coating layer applied, the adhesive, and the test dolly.

A test fixture, commonly referred to as a dolly, typically composed of aluminum, is attached to a properly prepared and cleaned surface using an adhesive compatible with the coating system, and with a rated strength (in psi or MPa) that exceeds the minimum test strength required for the test. After the adhesive cures sufficiently, the adhesion tester is mounted onto the dolly and a mechanical, hydraulic, or pneumatic device attempts to remove the dolly from the coated surface. Each component or layer involved in the test is designated according to an alphabetic naming convention detailed in the standard. The substrate is designated as location A, the first coating layer as B, the next coating layer as C, and so on. The adhesive or glue used to affix the dolly to the coated surface is referred to as Y, and the letter Z designates the test fixture or dolly. Three distinct types of failures are possible under ASTM D4541, including cohesion failure (failure within one distinct layer), adhesion failure (failure between two distinct layers), and glue failure. Under ASTM D4541, a glue failure may occur between the glue and

Above ASTM D4541 (Test Method E) showing 100% cohesive failure within the IOZ primer.

the test fixture, between the topcoat and the glue, or within the glue itself. A cohesion failure is identified by a single letter, which indicates the layer within which the failure occurred. For example, a 100% cohesive failure within the primer is reported as B- 100%. Two letters identifying an adhesion failure, (i.e., B/C), indicate the layers between which the failure occurred. The letter Y indicates a glue failure. The t hree genera l t y pes of test equipment cited in this standard are based on the means used to perform the pull (i.e., mechanical, hydraulic, or pneumatic). Each piece of equipment is designated within the standard as a Method using the letters B, C, D, E, and F. The Test Method (instrument) used for the test significantly affects the test result values. Tables showing results on four paint systems using dif ferent Methods are contained within the standard. T he t able s ac c ompa ny i ng t he

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standard show that tests conducted u s i n g t h e p n e u m a t i c e q u i p m e nt (Method D) and the hydraulic equipment (Methods C, E, and F) consistently achieve significantly higher test results than the mechanical portable adhesion tester (Met hod B). W hen repor ting results, ASTM D4541 requires reporting the instrument used to conduct the test. The increase in test values using t he pneumatic or hydrau lic testers, compared with the mechanical adhesion tester, is significant, often doubling the value obtained using the mechanical adhesion tester. Other factors affecting test result values include the following: (1) the degree to which the surface is prepared prior to attaching the dolly, (2) the method by which the dolly is prepared prior to affixing it to the surface, (3) the adhesive selected, including the surface temperature during the cure of the adhesive and the time interval between attaching the adhesive and performing the pull. Prior to attaching the dolly, the coated surface is cleaned in a manner that does not affect the coatings integrity and does not leave a residue. The standard allows for light abrading of the coating using 400-grit sandpaper or finer, followed by solvent cleaning to remove particulates from the abrading process. The solvent selected must not compromise the coatings integrity. Data published by DeFelsko on its Website found that how a dolly is prepared can result in a significant

difference in pull strength. The results indicate that preparing the dolly using Scotch-Brite pads resulted in an increased adhesion test value of 837 psi (5.77 MPa) compared to a machined dolly, and an increased adhesion value of 180 psi (1.24 MPa) compared to using sandpaper to abrade the dolly. M a ny d i f ferent ad he sive s a re u s ed for ad her i ng a dol ly to t he coated surface. Generally, solventless, two-component epoxies provide the best results. Different types of epoxies are available, including some fast-set epoxies that reach their full strength and can be tested within 1 hour after application. The drawback for some fast-setting epoxies is a reduction in t heir ma x imu m pu l l test st reng t h. Slower curing epoxies generally require a 24-hour cure time, but they also allow for higher psi testing, some up to 5,000 psi. Selecting an epoxy that cures at the anticipated surface temperature is critical. The time required between applying the adhesive onto the dolly and performing the pull test is a function of surface temperature and epoxy formulation. For tests performed in accordance with ASTM D4541, at least three tests are required in the area tested to statistically characterize the area. General reporting requirements include the following: (1) general nature of the test (field or lab), (2) temperature and relative humidity during the test period, (3) details regarding the test apparatus used, and (4) a description of each coat in the coating system. Specific requirements related to the

Above Cohesion, adhesion, and glue failures illustrating proper location designations in accordance with ASTM D4541.

test results include the following: (1) the date, test location, testing location, (2) the values, nature, and locations of the failures (using the location designations included in ASTM D4541), and (3) if scoring around the dolly was performed. Certain coatings types, such as inorganic zinc (IOZ) primers, typically fail cohesively. For example, in a threecoat system consisting of IOZ primer, epoxy intermediate coat, and polyurethane topcoat, the expected mode of failure is cohesive within the zinc primer. Therefore one should not be alarmed by a cohesion failure within the IOZ as long as the value at failure is at an acceptable level. Consult the coating manufacturer for its acceptance criteria.

AstM D6677
This adhesion test method uses a knife to determine the adhesion of a coating to a substrate or to another coating. Using a sharp knife, two cuts, each 1" (38.1 mm) in length, at a 300 to 450 angle, are made in the coating film, forming an X. The cuts must extend down to the substrate. The point of the knife is placed at the intersection of the cuts, and an attempt is made to lift the coating from the substrate or from other coating layers. Sufficient tests must be performed to ensure the adhesion evaluation is representative of the entire structure.

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Above Test s p er f or me d in close proximit y using different test methods as follows: Triangle (ASTM D6677), Circle (ASTM D3359), and Trapezoid (ASTM D4541).

ASTM D6677 conta i ns a sca le with ratings from 0 to 10. A rating of 10 indicates the coating is extremely difficult to remove with fragments no larger than approximately 1/32" by 1/32" (0.8 by 0.8 mm) removed with great difficulty. A rating of 0 indicates the coating can be easily peeled from the substrate to a length greater than " (6.3 mm). Ratings of 2, 4, 6, and 8 contain simi lar statements. The higher t he rating number, the more difficult the coating is to remove and the smaller the paint chips size removed. In accordance with ASTM D6677, any coating removed during the cutting process is to be disregarded. ASTM D6677 conta i ns severa l statements about the test method itself and about its relationship to ot her

adhesion test methods. These include the following: (1) this method is a qualitative and subjective test, (2) other adhesion test methods may be useful in obtaining quantitative results, and (3) no known correlation exists between this test method and other adhesion test methods, such as pull-off (ASTM D4541) or adhesion by tape (ASTM D3359). ASTM D6677 contains no precision and bias statement due to this test methods subjective character. Reporting requirements for ASTM D6677 include the following: (1) number of tests, (2) mean and range of the tests, (3) location of the failure (between the first coat and the substrate, between the first and the second coat, or within a coat), (4) structure tested, (5) location and environmental conditions at the time of the test.

ClOsinG reMArks
ASTM sta ndards a nd ot her industry standards are consensus standards w ritten w it h procedures, repor ting

requirements, and precision and bias statements. The purpose of the procedures within a standard is to ensure that different individuals perform the test following the same procedures and that they report the results using the same criteria. However, for some ASTM tests, such as ASTM D6677, no precision and bias statements are included since the test is subjective in nature. When an ASTM test method lists a rating scale, those who perform the test in accordance with the standard must employ the rating scale when reporting the results. Developing an independent rating scale that differs from the scale provided within the standard is not permitted. When a forensic investigator chooses to blatantly disregard the procedures and instructions contained within an ASTM standard and/or develops his or her own rating system, which benef its t he clients predetermined position, he or she is acting irresponsibly and not in accord with integrity required for conducting independent, fair investigations. cP
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