CCB 4423

Polymer Process Engineering

Laboratory Report

EXPERIMENT 6
PULL OFF ADHESION TEST

NURALIA SYAIRAH BT OSMAN 15669

NURUL FATIEHAH BT ABDUL HALIM 15592

1.0 INTRODUCTION
The experiment conducted is aimed to give students a better understanding on the concept of
coating adhesion and relate the effect of different curing time, curing temperature and effect
of water on the mechanical properties of the coating material. The technique used for this
experiment is the Pull off adhesion tester (ASTM D 4541) which is a method commonly used
to measure the coating adhesion. This test is able to quantify the strength of the bond between
substrate and coating.

2.0 MATERIAL AND EQUIPMENT

Epoxy

Steel plate

Elcometer 106 Pull Off Adhesion Tester (Scale 1,2,3,4 or 5)

Elcometer Acessories

20 Dollies

Pack of Araldite Adhesive

Magnetic Dolly Clamp

Dollu Cutter

Base Support Ring

Ratchet Spanner (Scale 3 and 4 only)

Polypropylene Carrying Case

3.0 PROCEDURE

1.

The surface of the dolly and the steel plates were cleaned by abrading it and ensuring
that it is free from oil, moisture and dust to ensure a good bond between the dolly and

2.

the surface.
The surface of the dolly was prepared and the coating where the dolly is to be applied
by roughening it with abrasive paper. These areas were then degreased by a suitable

3.

cleaning solvent.
A regular Araldite which is a two component epoxy paste was mixed and used within

4.

one hour. The two components were mixed in equal portion before applied.
For the first condition of curing, the adhesive was allowed to cure for about 1 hour at

5.

room temperature after being applied onto the dolly and the strength was measured.
For the second curing condition, 2 dollies were prepared and placed into an oven at

6.

120oC for 2 hours and the strength of the dolly was measured.
For the third condition, the second dolly immersed in water bath for 5 days and then

7.

the strength was measured.

After the curing process, the dolly were placed onto a test surface and pressure was

8.

applied.
The hand wheel or nut was slackened on the adhesion tester. The dragging indicator

9.

was set to zero (0) on the scale and the claw was engaged carefully with the dolly
The adhesion tester was held steadily with one hand to prevent rotation and tightened
the hand wheel and evenly applied increasing force to the dolly and thus stress was
also added onto the coating. This method was continued until the coating fails and the
dolly is removed from the surface or until the specified stress is reached .The value is

10.

read from the position of the dragging indicator after the test is complete.
According to the standards, the load should be applied uniformly. The hand wheel can
be turned in four or five stages to make a complete revolution. The wrench should be

11.

rotated without slipping

Before recording the results, the face of the dolly was inspected. In most cases the
coating will fully adhere to the dolly and the test can be claimed as 100% valid.
However, in some cases the coating will cover only part of the area of the dolly and a

12.

partial adhesion failure should be recorded.

If no coating is present on the dolly, this must be recorded as a failure of the adhesive.
This is normally due to incorrect or insufficient mixing of the components part of the

13.

adhesive or also due to the incompatibility of the adhesive and the coating
The test area was observed to give additional information about the type of failure:
adhesion and cohesion between different layers of the coating.

There are three curing conditions:

1. Curing for 2 hours at 120 C in oven and the strength is checked.

2. Curing for 24 hours at 80 C in oven and the strength is checked.

3. Curing for 24 hours at 80 C in oven and then it is immersed in water bath for 7 days.
The strength is then checked.
4.0 RESULTS
4.1 Report the relevant information as stated in ASTM D 4541.
ASTM D4541 is a standard method that define the procedures for evaluating and carrying
out pull-off adhesion testing of a coating on rigid substances such as metal, concrete or
wood. The test will determine either the greatest perpendicular force (in tension) that a
surface area can bear before a plug of material is detached, or whether the surface remain
intact a certain force (pass/fail). Pull-off adhesion testing is simply like any other tensile
testing but where the sample is very short.
Factor that need to consider when testing based on ASTMD4541.
-

Loading fixtures (or test elements or dollies) - The dollies must be cleaned sufficiently

to prevent "glue failure" during testing.

Rate of Pull Force Increase - Stress increase must be steadily incremental within the

rate intervals specified in ASTM D4541 / ISO 4624.

Pull stress must always be evenly distributed in the tested coating. If the pull stress is
not 100% evenly distributed throughout the pulled coating the area where the stress is

concentrated will fracture long before maximum stress has been reached elsewhere.
Use a "non-aggressive" adhesive which does not alter the coating chemically thereby
weakening it.
An adhesion test dolly is bonded to the coating using an adhesive. The Elcometer
106 and 108 adhesion tester houses a spring arrangement which applies a lift force to
the dolly as the tension is increased. When the coating is pulled off the surface, an
indicator on the scale shows the numerical value of adhesion expressed in terms of the
force per unit area required to remove the dolly. Inspection of the dolly face is required
to determine the failure mode.

4.2 Record the strength of your sample.

Elcometer 106
Trial 1
2 hours at oven 120C
7.5 MPa
(Fail too
small scale )
2 hours at Room
5 MPa (FAIL)
Temperature
1 week 120C
Test fail/Too
immersed in water
small scale
1 week Room
Test fail/Too
Temperature
small scale
immersed in water

Elcometer 108

Trial 2
-

Trial 1
7.5 MPa
(FAIL)

Trial 2
-

5 MPa
(PASS)
-

5 MPa (PASS)

4.5 MPa
(FAIL)
-

4.5 Mpa
(PASS)

4 Mpa (PASS)

4.3 Discuss the results and explain the difference between the cases.
In this experiment, Elcometer 106 and 108 are used for the same adhesive with
different curing conditions. In general, elcometer 106 gives lower pull-off strength
compared to elcometer 108. Elcometer 108 has higher efficiency compared to 106, based
on the observation on the surface after the pull-off test. Elcometer 106 leave adhesive
remaining on the steel plate while Elcometer 108 leaves clean surface after pull off test.
Things that are different is curing temperature. The result showed that dollies treated at
room temperature gives high pull-off strength compared to dollies treated in high curing
temperature. For samples that cured in water bath, the pull-off strength his lower for
Elcometer 106 and 108 compared to the samples at room temperature and oven. Wet
environments make the mechanical stability of composites bit low due to water sorption of
the matrix material. The hydrophilic groups of epoxy resins absorb water molecules that
alter the physical and mechanical properties of the resin. Water works as a plasticizer
leading to a softening of the adhesive. The interaction of absorbed water molecules also
cause decrease of mechanical properties and degradation of interface bonding
Impact of cure conditions:
-

Low cured temperature will result in slow cure and low crosslink density.
High cured temperature can cause high exotherms that may actually cause the system

to expand rather than shrink.

Proper cure conditions are dependent on the chemistry of the adhesives.

4.4 Give TWO (2) examples of application and discuss it.

Applications for the Elcometer 106 Adhesion Test include paint or plasma spray on bridge
decking, coatings on steel, aluminium, concrete etc. Two areas of applications includes
Chemical/Process Coating as well as Paint & Pigments.The Elcometer 108 Hydraulic
Adhesion Tester is an extremely versatile gauge which can be used for many adhesion
requirements. Adhesion tests can be made on flat or curved (concave and convex)
surfaces. Application includes coatings on Tanks, Pipelines, etc.The evaluation and
testing of adhesives is important as the adhesives can have different properties depending
on their volatile and non-volatile contents. The standards help to identify these properties
which include viscosity, adhesion, shear strength, and shear modulus. The adhesives are
utilized to form bonds or joints between adherend materials which can be metal, wood, or
plastic. The standards also help to identify adhesive bond or joint mechanical properties
which include strength, creep, fracture, and fatigue. The different effects of environmental
factors on adhesive bonds and joints are also evaluated. The adhesives standards are
instrumental in determining various applications of adhesives such as in electrical
insulation, sealing materials, and materials used in lumber products and floor systems.
5.0 CONCLUSION
ASTM's adhesives standards are helpful in the evaluation and testing of adhesives. The
test determines either the greatest perpendicular force (in tension) that a surface area can
bear before a plug of material is detached, or whether the surface remains intact at a
prescribed force (pass/fail). Failure will occur along the weakest plane within the system
comprised of the test fixture, adhesive, coating system, and substrate, and will be exposed
by the fracture surface. This test method maximizes tensile stress.

REFERENCES
http://www.dfdinstruments.co.uk/topics/Study5-ASTM-D4541.htm