Corrosion & Prevention 2013 Paper 115 - Page 1

RECENT DEVELOPMENTS IN THE TESTING

OF COATING ADHESION

JF. Fletcher
1
& CL. Bennett
1

1
Elcometer Limited, Edge Lane, Manchester, M43 6BU, UK

SUMMARY: Adhesion testing of coatings can be divided in to two methods, the cross-cut method
and the tensile pull-off method. There are international standards detailing both of these techniques.
However, recent changes in these standards need to be described and discussed.

ISO 2409: Paints and Varnishes Cross-cut test, has been revised and now has a 2013 publication
date, while the ASTM D3359: Standard Test Methods for Measuring Adhesion by Tape Test, has
also been revised and was submitted for ballot in May 2013. Both of these revisions contain
significant changes particularly with respect to the issue of the tape used to remove loose coating
after cutting.

ISO 4624: Paints and Varnishes Pull-off test for adhesion was published in 2004 and BS EN ISO
16276-1: Corrosion protection of steel structures by protective paint systems assessment of, and
acceptance criteria for, the adhesion/cohesion (fracture strength of a coating part 1 pull-off testing,
was published in 2007 and describes the field assessment of adhesion/cohesion with guidance for
the interpretation of the results and acceptance/rejection criteria.

ASTM D4541, Standard Test Method for Pull-Off Strength of Coatings Using Portable Adhesion
Testers describes five different types of pull-off tester and there has been a recent round robin trial
carried out using all of these methods.

ASTM D7234, Standard Test Method for Pull-Off Adhesion Strength of Coatings on Concrete
Using Portable Pull-Off Adhesion Testers has also been the subject of a recent round robin.

In addition there is a new design of pull-off adhesion tester and this paper will describe the test
results for protective coatings on blasted steel substrates.

Keywords: Adhesion, Testing, Coatings, Standards.

1. INTRODUCTION

Field testing for the adhesion of protective coatings can be divided in to two test method types, the Cross-Cut (X-Cut)
Method and the Tensile Pull-off Method. BS EN ISO 16276, Corrosion protection of steel structures by protective paint
systems - Assessment of, and acceptance criteria for, the adhesion/cohesion (fracture strength) of a coating has two
parts. Part 1 describes the Pull-Off test method and Part 2 describes the Cross-cut method.

The ASTM Standard Test Methods for measuring adhesion by tape test is D3359 and the equivalent ISO Method is ISO
2409, Paints and Varnishes Cross-cut test.

The Tensile Pull-off method is described in ASTM D4541 and ISO 4624, with a specific ASTM method for testing
coatings on concrete contained in D7234.

As BS EN ISO 16276 covers both Cross-cut and Pull-off methods the basics of the Cross-cut method are described
below, but this paper mainly deals with the operation of the Pull-off method.


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2. THE CROSS-CUT METHODS

In BS EN ISO 16276-2 the procedure for rating the resistance of coating systems when a cut in the form of a right-angle
lattice pattern (cross-cut) or in the form of an X (X-cut) is made into the coating, penetrating through to the substrate is
given. This standard also specifies suitable equipment and defines inspection areas, sampling plans and
acceptance/rejection criteria. It does not specify ratings for particular coating systems. The standard references both ISO
2409 and D3359 for the cross-cut and X-cut methods. Figure 1 shows a typical cross-hatch cutter and figure 2 shows the
rating chart for the cross-hatch pattern.



Figure 1 The Cross-hatch Adhesion Test Kit
Showing the Handle with Blade Fitted, the Magnifier and the Adhesive Tape. The insert shows a Magnified Image
of the Cutter Blade


The spacing of the cuts is dependent on the thickness of the coating to be measured and the cutter sizes are given in
table 1 below. The brush and tape are used to prepare the matrix for visual inspection using the X10 magnifier.

It should be noted that the ISO and ASTM ratings systems are reversed with respect to each other, as shown in figure 2.
In the ISO method, the rating of 0 (zero) equates to no damage caused by the cuts and the rating of 5 equates to the
maximum damage. For the ASTM method, the rating of 0B is maximum damage (no adhesion) and the rating 5B is no
damage (maximum adhesion). The letter B in the ASTM rating relates to method B within D3359 with method A being
the X-cut method.

It is also the case that the adhesive tapes mentioned in the ISO and ASTM methods are different and are applied and
removed using different techniques. It should be noted that the 2013 version of BS EN ISO 2409 does not define the
tape by size or by adhesion specification.

Table 1 Cross-cut Blade Sizes by Thickness Range



Number of Cutting Edges Spacing (mm) Coating Thickness Range
(m)

Relevant Standard
11 1.0 0 50 ASTM only
6 1.0 0 60 ISO only
11 1.5 0 60 ASTM only
6 2.0 0 60 ASTM only
6 2.0 50 125 ASTM only
6 2.0 61 120 ISO only
6 3.0 125 250 ISO & ASTM
Corrosion & Prevention 2013 Paper 115 - Page 3


Figure 2 The Cross-hatch Rating Systems for both the ISO and ASTM Methods

The X-cut method calls for an X-cut in the form of a St Andrews Cross to be made through the coating using a sharp
blade. The angle between the cuts should be between 30 and 45 and should be approximately 40 mm long. Adhesive
tape is applied with a firm force and pulled off to remove any loose coating. The adhesion is rated using the scale shown
in figure 3.



Figure 3 An Example of a Cross-cut Rating Scale
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3. PULL-OFF ADHESION TESTING

BS EN ISO 16276-1 describes procedures for assessing the fracture strength of a coating system using the pull-off
method. Test cylinders, often called dollies, are fixed to the surface of the coating using a suitable adhesive and a
force is applied in order to cause a fracture in the coating beneath the dolly. The equipment measures the force required
to fracture the coating and it is reported in terms of force per unit area, e.g. MPa (psi). The standard also defines
inspection areas, sampling plans and acceptance/rejection criteria for the pull-off adhesion test.

ASTM D4541 describes a procedure for evaluating the pull-off strength of a coating system and recognises that this is
commonly referred to as adhesion. The test determines either the greatest perpendicular force that a coated surface can
bear before a plug of material is detached or whether or not the coating remains intact when a prescribed force is
applied. Failure will occur at the weakest part of the coating system be that the steel substrate/primer coating interface,
the intermediate coating to primer interface, other coating interfaces or even within a coating layer.

It should be noted that for both the ISO and ASTM methods, inspection of the face of the dolly after it has been pull-off
the surface is crucial to the procedure and to the reporting of the outcome.

Test method D4541 was originally developed for coatings on metal substrates, but it may be appropriate for other rigid
substrates such as plastic and wood. The test user and the person or organisation specifying the use of this test should
address issues such as the loading rate and the flexibility of the substrate when preparing to use this test method.

The test method uses a class of test instruments known as portable pull-off adhesion testers that are capable of exerting
a force on the dolly and a counter force on the surface of the coating so that the test can be carried out when only one
side of the coated sample is accessible.

There are five different types of test instruments described in the method and it is recognised that, as the force that is
applied to the dolly stresses the coating in different ways, comparisons between the results using different types of test
instruments is not possible.
There are some aspects of pull-off adhesion testing that are common to all the types of instruments, such as the rate at
which the force should be applied. Both BS EN ISO 16276-1 and ASTM 4541 specify a rate of 1 MPa/s or less for a 20
mm diameter dolly, so that the pull testing is completed within 100 s or less. Also the force should be applied in as
continuous and smooth a manner as is possible. The dolly should not be subjected to any distortion or misalignment
before or during the test to avoid additional stress on the coating.

This raises the issue of cutting round the dolly, which is generally left to the user of the test to decide. It is known that
for certain types of coating cutting the coating round the dolly to isolate the area of the coating under the dolly can
cause micro-fissures to propagate in the coating under the dolly reducing the adhesion performance. However, other
types of coatings, such as elastomers, show the effect of the surrounding coating supporting the coating under the dolly
unless the coating is cut through round the dolly. This is a decision that required detailed knowledge of the coating and
should therefore be arrived at in consultation with the coating manufacturer.

Test method D7234 describes a similar method for the determination of the pull-off strength of coatings on concrete.


4. TYPES OF PORTABLE PULL-OFF ADHESION TESTERS

Portable adhesion Testers can be operated by compressed spring assemblies, hydraulic pressure or pneumatic pressure
and there are several different designs available for the different types. The five types of equipment described in D4541
are detailed as follows:

Fixed Alignment Adhesion Tester Type II

Self-Alignment Adhesion Tester Type III

Self-Alignment Adhesion Tester Type IV

Self-Alignment Adhesion Tester Type V

Self-Alignment Adhesion Tester Type VI

Corrosion & Prevention 2013 Paper 115 - Page 5
The Type I tester originally described in D4541 was used for testing coatings on concrete and has been taken out of this
test method and put in to the D7234 test method for the testing of adhesion of coatings applied to concrete.

The Type II tester is the mechanical pull-off adhesion tester shown in figures 4 and 5, where the force is generated by
compressing a helical spring or a set of spring washers depending on the scale range of the unit.




Figure 4 The Fixed Alignment Adhesion Tester Operated by a
Compressed Spring, Showing the 20 mm dollies, the support
ring, 2-pack adhesive, Cutter and Magnetic Clamp for Steel
Substrates.
Figure 5 The Fixed Alignment Adhesion Tester
Operated by a Compressed Washers, Showing the
20 mm dollies, the support ring, 2-pack adhesive,
Cutter and Magnetic Clamp for Steel Substrates.

The Type III tester is the Hydraulic Adhesion Tester, sometimes called the HATE Adhesion Tester, originally
developed for testing coatings for North Sea Off-Shore applications and operated using a hydraulic piston pushing a pin
through the stainless steel dolly to push the coated substrate of the dolly. Figure 5 illustrates this type of adhesion tester.






Figure 6 The Hydraulic Self Alignment Hydraulic
Adhesion Tester Showing the Analogue and Digital
Versions.

Figure 6 Convex and Concave Curved Dollies
For the Hydraulic Adhesion Tester

The Type IV tester is operated pneumatically used either a compressed gas line or a small CO
2
cylinder to charge the
gas reservoir. There are several versions of this type of tester all using a range of piston sizes to achieve the range of
pull force up to 70 MPa. Figure 7 illustrates one of these testers with a PC operated microscope for inspecting and
recording the condition of the face of the dolly and a data output for recording the force vs. time characteristic for the
pull test.

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Figure 7 The Pneumatic Self-Alignment Adhesion Tester
Showing the CO
2
Cylinder on Top, the PC Microscope on the Left
And the Piston in the Centre
Figure 8 The Piston Assembly Ready for Testing

The Type V tester is also operated by hydraulic pressure but the self-alignment method for the connection to the dolly is
different to that of Type III and is illustrated in figure 9.



Figure 9 Schematic Illustration of the Self-Alignment Mechanism for the Type V Tester.

A new form of the Type V adhesion tester has been introduced and this design has analogue and digital pressure gauge
options, pre-calibrated so that the user can choose between 20 mm and 14.2 mm diameter dollies for testing coatings on
metals surfaces or the 50 mm diameter dolly for testing coatings on concrete. The 14.2 mm dollies have a surface area
that is very close to half that of the 20 mm dollies, within 1 %.






Figure 10 The New Hydraulic Adhesion Tester with Digital Gauge
and 14.2 mm, 20 mm and 50 mm Diameter Dollies
Figure 11 Dolly Pull-off Mechanism Ready For
Testing

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Test Dolly
Adhesive
Topcoat
Primer
2nd coat
Intermediate coats
Substrate
Adhesive: Adhesive/Test Dolly
Cohesive: Adhesive
Adhesive: Topcoat/Adhesive
Cohesive: Topcoat
Adhesive: Intermediate/Topcoat
Cohesive: Intermediate
Adhesive: 2
nd
Coat/Intermediate
Cohesive: 2
nd
Coat
Adhesive: Primer/2
nd
Coat
Cohesive: Primer
Adhesive: Substrate/Primer
Cohesive: Primer
Adhesive: Adhesive/Test Dolly
Cohesive: Adhesive
Adhesive: Intermediate/Topcoat
Adhesive: Topcoat/Adhesive
Adhesive: 2
nd
Coat/Intermediate
Cohesive: Intermediate
Adhesive: Primer/2
nd
Coat
Cohesive: 2
nd
Coat
Adhesive: Substrate/Primer
Cohesive: Topcoat
Cohesive: Primer
The new Hydraulic Adhesion Tester has an easy to use piston mechanism with gearing to make it simple to achieve the
required rate of increase of the pull-off force. Different skirts are available for the different diameter dollies and for thin
substrates.

The Type VI tester has yet another design for the achievement of self-alignment. In this case, the four legs of the test
head that fits on to the dolly operate independently driven by the hydraulic pressure generated by the hand cranked
pump. Figure 12 shows this type of tester with a range of dollies of different sizes and configurations. It should be noted
that this design deals with uneven substrates such as curved surfaces or steps by allowing each leg to take up the
difference without changing the orientation of the pull force. The Type V method illustrated above does still have a
tendency to exert a peeling moment to the dolly if the adhesive layer is formed as a wedge.




Figure 12 The Type VI Adhesion Tester Figure 13 The Principle of the Self-
Alignment Head for the Type VI Tester.





















































Figure 14 Description of the types of fracture

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5. INSPECTION AREAS AND SAMPLING PLANS

BS EN ISO 16276-1 states that the inspection areas will normally be defined in the project specification. This applies to
both new constructions and the surveying of existing structures. However, if the structure has not been divided in to
individual inspection areas then the whole structure is considered as the inspection area. It is also recommended that
areas where the adhesion specification is difficult to achieve should be considered as individual inspection areas. This
ensures that an area of low adhesion does not cause the whole of the project to be rejected.

Random measurements are made according to the table of minimum numbers of readings within an inspection area
given in the standard. For example, if the inspection area is < 1,000 m, there should be 3 valid measurements for every
250 m area or part thereof. For areas > 1,000 m, there should be 12 valid measurements plus 1 additional valid
measurement for every additional 1,000 m. It is recommended that such areas be subdivided in to smaller inspection
areas.

6. INTERPRETATION AND EXPRESSION OF THE RESULTS

All the pull-off adhesion test standards recognise that the type of failure is significant and should be reported. First and
foremost, a glue failure is not a valid reading unless the force applied to achieve the failure value is above the value
specified, in which case the coating can be said to have exceeded the adhesion specification.

Normally a glue failure with be an invalid test and the test will have to be repeated unless allowance for possible glue
failures has been included in the number of dollies applied to an inspection area. When the force exceeds the specified
value it is not necessary to continue until the coating fails, as that will require a repair to the coating and such a test will
not provide any additional information.

If the fracture strength is less than the specified value the validity of the test is determined by visually inspecting the
face of the dolly and determining the area of the coating failure. If more than 20% of the area of the face of the dolly
shows failure of the adhesive and or cohesive failure of the glue or adhesive failure at the adhesive/topcoat interface the
test is not valid. For a fracture to be identified as adhesive or cohesive the area of the relevant fracture must be 80% or
more of the dolly face.

Figure 14 shows the schematic descriptions of the types of fractures that can occur when pull-off testing a protective
coating system. Valid tests require the conditioning of the coating to be according to ISO 4624, i.e. temperature of 23
2 C and relative humidity of 50 5% for 16 hours prior to the test. If these conditions are not achieved that laboratory
testing according to ISO 4624 shall be carried out. In general, such conditions will not be achieved in the field unless
the area to be tested is protected by some form of encapsulation.

In 2009 a round robin assessment of ASTM D4541 was carried out to compare the results from different operators,
testing on different coatings using the five different adhesion tester types. This testing was carried out to prepare a
precision statement for inclusion in the standard so that users would be able to see how the results they obtain using the
method compare with the results obtained in the round robin. As there are no accepted reference materials it is not
possible to prepare a bias statement for the method.


7. TESTING ISSUES

The main practical issues in respect of adhesion testing are around the choice and use of the adhesive. It is common
practise for the manufacturer of the adhesion tester to supply an adhesive in the kit so that the user can start testing as
soon as the adhesion testing kit is delivered. However, the general purpose adhesive supplied may not be optimised to
the testing to be done. Those most able to comment and recommend suitable adhesives are the formulators of the
coating as they will know what adhesives are compatible with their coating.

The main issue with general purpose adhesives is the cure time. The commonly-used twin-pack epoxy adhesives are a
rugged and easy to use but they typically takes 16 hours to cure at ambient temperatures. These adhesives are easy to
mix and the proportions of resin to hardener are not critical to getting a full strength bond. Work on testing the adhesion
of high temperature resistant coatings such as vitreous enamel show that when the twin-pack adhesives are applied to
heated panels at about 100C they can achieve sufficient strength to pull coatings off at about 5 MPa in 20 to 30
minutes. This can be equivalent for the panel to cool to 25 to 30C but there are few paint coatings that will not be
affected by such temperatures.

Another commonly used adhesive type is the Cyanoacrylate glue, which is much quicker to cure but requires very clean
surfaces to bond to their full strength. Some paint coatings are adversely affected by these adhesives and coatings such
Corrosion & Prevention 2013 Paper 115 - Page 9
as flame sprayed aluminium or zinc allow the low viscosity adhesive to penetrate their structure adding to the
uncertainty of the adhesion test.

The issue of glue failure is a major problem to users of the adhesion test particularly when a certain number of tests
must be carried out to adequately determine the adhesion in a given inspection area. For example, if 12 valid tests are
required how many dollies should be applied, 14, 16 or more?

One of the practical aspects for the choice of the adhesive is the cure time. The most commonly used twin-pack epoxy
adhesives take 16 hours to fully cure at room temperature. While raising the temperature will increase the cure rate and
therefore reduce the time between gluing the test dolly to the surface and applying the pull-off force, there are few
coatings that will not be affected by raising the temperature more than a few degrees. One coating that can be tested
after curing the adhesive at elevated temperatures in vitreous enamel.

Even the Cyanoacrylate glues take several hours to achieve their full strength. For example, the adhesive supplied for
use with the Hydraulic Adhesion Tester takes at least 2 hours to reach a satisfactory level of adhesion for testing some
coatings. However, the data sheet states that the time required to reach full strength is 24 hours.

The precision statement contained in D4541 was determined in a round robin study (Interlaboratory study, ILS) carried
out in 2007 when analysts (operatives) from seven laboratories tested six different coatings applied to 6 mm (") thick
hot-rolled steel plates using five different adhesion testers. Every individual determination was treated as a single test
result. Any pull which exceeded the testers upper limit and any pull where there was 50% or more glue failure were
eliminated from the statistical analysis. If four pulls were obtained from an operator for a particular coating, the fourth
pull was eliminated and the first three pull values were included in the statistical analysis.

Six different coatings were used as a means to achieve a range of pull-off strengths covering the operating range of all
the instruments included in the testing. It should be noted that two of the coatings, Coating A and Coating F produced
results that exceeded the upper limits of the adhesion testers available for the testing and results for these two coatings
were eliminated from the statistical analysis. In practise higher adhesion testing ranges for some of the equipment can
be obtained by either reducing the diameter of the test dolly or increasing the pull force, for example; by increasing the
size of the piston used for the Type IV Tester.

D4541 expresses the results in five separate tables, one for each adhesion tester type and the repeatability limits are
given in these tables. Table 2 below shows the reproducibility standard deviation for all the data for each of the
adhesion tester types averaged across the coating types, B to E. This extract from the full table 6 contained in D4541
shows the maximum expected difference between values achieved by a single operator using equipment from the same
type. Two readings taken on the same coating by the same operator should be considered suspect if they differ by more
than the percentage difference stated.

Table 2 Precision of Pull-Off Measurements by Adhesion Tester Type

Adhesion Tester Type Test Method Maximum Recommended
Difference (%)
Type II B 64.7
Type III C 33.8
Type IV D 14.8
Type V E 27.8
Type VI F 17.5


8. CONCLUSIONS

The field testing of the adhesion properties is an important method for testing coatings on both new construction and
structures that have been in service for some time. The adhesion requirement for a coating system is often included in
the specification for the work and usually stated on the coating manufacturers datasheet. The Cross-Hatch or Cross-Cut
methods provide a rating of the coating adhesion and this can be useful when surveying a coating that has been in
service for some time in order to asses if a repair is required. The pull-off test provides a method that measures the
adhesion in terms of the force per unit area that is required to fracture the coating. The pull-off test can be applied to
new coatings that are fully cured as an acceptance test or to coatings that have been in service.

The standards provide test methods that allow the tests to be uniformly applied by defining the preparation, testing,
evaluation and reporting of the pull-off adhesion tests. ASTM D4541 describes five different types of portable adhesion
Corrosion & Prevention 2013 Paper 115 - Page 10
tester and BS EN ISO 16276-1 references D4541 and ISO4624 and also defines inspection areas, sampling plans and
acceptance/rejection criteria for the pull-off adhesion test.

To achieve reliable test results the adhesive used to apply the test dolly to the surface of the coating needs to be chosen
carefully so that it does not have any effect on the coating during the application and cure process. Any adhesive can be
used to stick the test dolly to the surface of the paint coating but it should have an adhesion performance that exceeds
the performance of the coating for valid results to be achieved.

A smooth and uniform application of the force applied to the coating is very important to the consistency of pull-off
testing as uneven force application can stress the coating in unpredictable ways causing premature pull-off values.

When testing a structure it is important to agree the type of equipment to be used for the test, as the different equipment
types apply the force to the test dolly in different ways and this means that different failure mechanisms can occur in the
coating. Results from different types of test equipment cannot be compared directly.

9. AUTHOR DETAILS



John Fletcher has been with Elcometer Limited in Manchester since 1982 and
he is registered as a Chartered Scientist. He is currently the Technical Support
Manager, a position he has held since 1998. He is responsible for Customer
Support, Product Training, Compliance to Standards and QA. He is a Fellow of
the Institute of Corrosion and is currently Vice President of ICorr.


Colin Bennett is the Regional Sales Manager at Elcometer Limited in
Manchester, a position he has held since 2004. He is responsible for sales of
Elcometer product in a number of world regions including South America,
Japan and Australia/New Zealand.