f l u I ‘ J I

INTERNATIONAL ORGANIZATION FOR STANDARDIZATION~MEKLlYHAPO/lHAR OPTAHMSAUHR il0 CTAHLiAFTH3AUMH.ORGANISATION INTERNATIONALE DE NORMALISATION

Paints and varnishes - Pull-off test for adhesion

Peintures et vernis - Essai de traction

First edition - 1978-07-01

~~

UDC 667.613 : 620.179.4 Ref. No, IS0 4624-1978 (E)

Descriptors : paints, varnishes, tests, tension tests, test equipment.

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FOREWORD
I S 0 (the International Organization for Standardization) is a worldwide federation
of national standards institutes ( I S 0 member bodies). The work o f developing
International Standards is carried out through I S 0 technical committees, Every
member body interested in a subject for which a technical committee has been set
up has the right to be represented on that committee. International organizations,
governmental and non-governmental, in liaison with ISO, also take part in the work.

Draft International Standards adopted by the technical committees are circulated

to the member bodies for approval before their acceptance as International
Standards by the I S 0 Council.

International Standard I S 0 4624 was developed by Technical Committee

ISO/TC 35, Paints and varnishes, and was circulated to the member bodies in
August 1976.

It has been approved by the member bodies of the following countries :

Australia Germany Poland
Austria India Portuga I
BeIgium Iran Romania
Brazil Israel South Africa, Rep. of
Bulgaria Korea, Rep. of Sweden
Canada Mexico Switzerland
Chile Netherlands Turkey
Czechoslovakia New Zealand United Kingdom
Egypt, Arab Rep. of Norway Yugoslavia
France Peru

The member body of the following country expressed disapproval of the document
on technical grounds :
Italy

O international Organization for Standardization, 1978 0

Printed in Switzerland
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 Paints and varnishes - Pull-off test for adhesion

O INTRODUCTION 1 SCOPE AND FIELD OF APPLICATION

This International Standard i s one of a series of standards This International Standard specifies methods for carrying
dealing with the sampling and testing of paints, varnishes out a pull-off t e s t on a single coating or a multi-coat system
and related products. It should be read in conjunction with of paint, varnish or related product.
I S 0 1512, I S 0 1513, I S 0 1514and I S 0 2808.
The test may be applied using a wide range of substrates.
Different procedures are specified according to whether the
This International Standard specifies a method for assessing
substrate is deformable, for example thin metal, plastics
the adhesion of a single coating or a multi-coat system of
and wood, or rigid, for example thick concrete and metal
paint, varnish or related product by measuring the mini- plates. For special purposes, the coating may be applied to
mum tensile stress necessary to detach or to rupture the a test cylinder and, in this case, a method for determina-
coating in a direction perpendicular to the Substrate.
tion of the coating thickness shall be agreed between the
interested parties.
The t e s t result is influenced not only by the mechanical
properties of the system under test, but also by the nature The test result i s the minimum tensile stress necessary to
and preparation of the substrate, the method of paint break the weakest interface (adhesive failure) or the weakest
application, the drying conditions of the coating, tempera- component (cohesive failure) of the test assembly. Mixed
ture, humidity and other factors. adhesivehohesive failures may also occur,

The method o f t e s t specified below requires to be com- 2 REFERENCES

pleted, for any particular application, by the following
supplementary information. This information should be IS0 1512, Paints and varnishes - Sampling.
derived from the national standard or other document for I S 0 1513, Paints and varnishes - Examination and prep-
the product under t e s t or, if appropriate, shall be the aration of samples for testing.
subject of agreement between the interested parties.
IS0 1514, Paints and varnishes - Standard panels for
a) Material and surface preparation of t e s t assembly testing.
surface or substrate. I S 0 2808, Paints and varnishes - Determination of film
b) Method of application of t e s t coating to the thickness.
substrate or test cylinder, if appropriate.
3 APPARATUS
c) Duration and conditions of drying of the coating
(or conditions of stoving and ageing, if applicable] 3.1 Tensile tester, suitable for carrying out the chosen
before testing. procedure specified in clause 7. The tensile stress shall be
applied in a direction perpendicular to the plane of the
d) Thickness, in micrometres, of the dry coating, coated substrate and shall be increased a t a substantially
including the method of measurement in accordance uniform rate, not greater than 1 MPa/s*, such that failure
with I S 0 2808, and whether it i s a single coating or a of the test assembly occurs within 90 s. Suitable designs
multi-coat system. for applying the tensile stress are shown in figures 1 and 2.
e) The adhesive (and mixing ratios, if applicable) and
curing conditions (see also clause 4). 3.2 Test cylinders, suitable for use with the tensile
tester (3.11, steel faced, of diameter 20 mm (unless other-
f ) Duration and conditions between assembly and wise agreed) and of sufficient thickness to ensure freedom
testing. from distortion during the test. It i s recommended that the
g) Type of pull-off t e s t assembly used (see 7.3).
length of the t e s t cylinder should be not less than half i t s
diameter. The faces shall be machined perpendicular to the
h) Type of tensile tester and diameter of test cylinder. long axis of the cylinder before use.

* 1 MPa/s = 1 MN/m2.s
~ -_-__I_

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 IS0 4624-1978 (E) 4624-78

. .._

FIGURE 1 - Example of a suitable test apparatus for methods specified in 7.3.1 and 7.3.3

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 eI

Test piece
Coating
Test cylinder

Ball-and-socket
sliding joint

Support (suitably
designed to allow
for joint assembly)

Ball -and-socket
sliding joint

FIGURE 2 - Example of a suitable test apparatus for method specified in 7.3.2

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 IS0 4624-1978 (E) 4 624-78 1 4 8 5 1 9 0 3 0034970 7

3.3 Centring device, for ensuring proper coaxial alignment 5 SAMPLING

of the test assembly during the adhesion process used as
Take a representative sample of the product to be tested
described in 7.3.1 and 7.3.3. A suitable design is shown in
(or of each product in the case of a multi-coat system) as
figure 3.
specified in IS0 1512. Then examine and prepare the
sample for testing as specified in I S 0 1513.
3.4 Cutting device, such as a sharp knife, for cutting
through cured adhesive and the paint coating to the
substrate, round the circumference of the t e s t cylinder.

6 TEST SUBSTRATES
4 ADHESIVES
Special attention i s required in selecting suitable adhesives 6.1 Preparation and coating of test substrate
to be used in the test.
Prepare the specified test substrate in accordance with
To produce failure of the coating, it i s essential that the IS0 1514 and then coat it by the specified method with the
cohesive and bonding properties of the adhesive be greater product or system under test.
than those of the coating under test.
Preliminary screening of adhesives shall be carried out
in order to determine their suitability for use. Suitable 6.2 Drying the test coating
adhesives and, if applicable, their unmixed components
shall cause l i t t l e or no visible change in the coating under Dry (or stove and age) the coated test substrate for the
t e s t when l e f t in contact with the coating for a period specified time and under the specified conditions and
equivalent to the curing time of the adhesive. condition it a t 23 f 2 O C and (50f 5) % relative humidity
for a minimum of 24 h. Then carry out the appropriate
An adhesive may be considered suitable for a particular t e s t procedure as soon as possible.
coating if it gives the same test result as that produced by
using a different class or type of adhesive when similarly
tested.
6.3 Thickness of coating
NOTE - In most cases, cyanoacrylate, two-component solventless
epoxide and peroxide-catalysed polyester adhesives have been found Determine the thickness, in micrometres, of the dry coating
suitable. Cyanoacrylate and polyester adhesives have a short curing
time and are preferred for use with coatings that have been sub- by one of the procedures specified in I S 0 2808. See also
jected to highly humid conditions. clause 1.

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 I S 0 4624-1978 (E)

7 PROCEDURE 7.3.2 Method for testing from one side only (suitable for
rigid substrates only)
7.1 Ambient conditions Apply the adhesive evenly to the uncoated, freshly-cleaned
Carry out the test a t 23 f 2 O C and *
(50 5) % relative surface of a test cylinder (3.2). Place the adhesive-coated
face of the t e s t cylinder in contact with the coating, (see
humidity.
note 1 in 7.3.11, for a period equal to the curing time of the
adhesive (see note 2 in 7.3.1). A t the end of this period,
carefully use the cutting device (3.4) to cut around the
7.2 Adhesives
circumference of the t e s t cylinder through to the substrate,
Prepare and apply the adhesive in accordance with the
Place the outer ring in position and t e s t as indicated in
manufacturer's instructions. Use the minimum quantity of
figure 5.
adhesive required to produce a firm, continuous and even
bond between the components of the test assembly. Outer ring
Remove any excess adhesive immediately if possible.

Test cylinder coated

with adhesive
7.3 Test assemblies
Paint coating

7.3.1 General method for testing both rigid and Coated substrate
deformable substrates
Use as the t e s t piece an area, cut from the coated substrate FIGURE 5 - Test assembly for rigid substrates
(disc of minimum diameter 30 mm or square of minimum
side 30 mm). Take care not to distort the test piece. Apply 7.3.3 Method using test cylinders
the adhesive evenly to the surfaces of two freshly-cleaned
test cylinders (3.2) of equal diameter (see notes 1 and 3). Apply the adhesive evenly t o the uncoated, freshly-cleaned
Place the test piece between the adhesive-coated faces of surface of a t e s t cylinder. Place the adhesive-coatedsurface
the t e s t cylinders such that the test cylinders are coaxially of the t e s t cylinder in contact with the surface of the
aligned in the centre of the piece, as shown in figure 4. cylinder coated with the product under test, as shown in
Align the t e s t assembly in the centring device (3.3) and figure 6, and align the t e s t assembly in the centring device
maintain the alignment for a period equal to the curing (3.3) for a period equal to the curing time of the adhesive.
time of the adhesive (see note 2). At the end of this period,
carefully use the cutting device (3.4) to cut around the
circumference of the test cylinders through to the substrate.
Painted test cylinder
Paint film

t Adhesive
Test cylinder coated

I + Test cylinder coated

with adhesive
with adhesive

Substrate painted
on one or both sides FIGURE 6 - Test assembly using test cylinders

Test cylinder coated

with adhesive 7.4 Measurement
Immediately after the period allowed for the curing of the
adhesive, place the t e s t assembly in the tensile tester (3.11,
taking care to align the t e s t cylinders so that the tensile
FIGURE 4 - Test assembly, sandwich method force is applied uniformly across the test area, without
(substrate painted on one or both sides) bending moment. Apply a tensile stress, increasing a t a rate
not greater than 1 MPa/s, perpendicular t o the plane of
the coated substrate such that failure of the t e s t assembly
NOTES shall occur within 90 s of initial application of the stress.
1 The adhesion at the adhesive coating interface may be improved
b y lightly abrading the surface of the dried coating before appli- Record the tensile stress to break the t e s t assembly and
cation of the adhesive-coated face of the test cylinder. examine the fracture surfaces in accordance with 9.2.
2 In special tests under highly humid conditions, the curing time
of the adhesive shall be as short as possible. 7.5 Number of determinations
3 In the method for deformable substrates, if a poor adhesive bond
is expected between the uncoated face of the substrate and the test
Carry out a t least three determinations. For referee
cylinder, coat both faces of the substrate with the product under purposes, carry out a minimum of five determinations.
test. Report the results of all determinations.

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 8 NOTES ON PROCEDURE A/B = Adhesive failure between substrate and first coat

8.1 The results may be influenced by the test assembly B = Cohesive failure of first coat
used. Furthermore, the results are not reproducible unless
B/C = Adhesive failure between first and second coats
coaxial alignment of the tensile forces is ensured.
-/Y =Adhesive failure between final coat and adhesive

8.2 Where failure is mainly associated with the adhesives, Y = Cohesive failure of adhesive
the use of another type of adhesive may enable more useful Y/Z = Adhesive failure between adhesive and test
re.sults to be obtained. cylinder
Example : If a paint system tested in the pull-off test
breaks a t a tensile stress of 20 MPa and examination of the
9 EXPRESSION OF RESULTS area on each side of the site of separation reveals approxi-
mately 30% of the test cylinder area associated with
cohesive break of the first coat and 70% of the test
9.1 Breaking strength
cylinder area associated with intercoat adhesive break
The breaking strength, in megapascals, for each test between the first and second coats, the pull-off test result '
assembly is given by the formula i s expressed as

-
4F 20MPa, 3 0 % B, 70%B/C
nd2
where 10 TEST REPORT

F i s the breaking force, in newtons; The test report shall contain a t least the following infor-
mation :
d i s the diameter, in millimetres, of the t e s t cylinder.
a) the type and identification of the product(s) tested;
In the case of t e s t cylinders of diameter 20 mm, the break-
ing strength, in megapascals, is given by the formula b) a reference to this International Standard or to a
corresponding national standard;
4F --F
--
c) the items of supplementary information referred to
40On 314
in the Introduction to this International Standard;
d) a reference to the national standard or other docu-
9.2 Nature of failure ment supplying the information referred to in c) above;
Express the result as the percentage area and site of fracture e) the result of the test, reported as required in 9.1
in the system under t e s t in terms of adhesive, cohesive or and 9.2 (together with any further details required by
adhesive/cohesive failure. t h e document referred to in c) above);

For convenience, the following scheme may be used to f) any deviation, by agreement or otherwise, from the
describe the results observed, procedure specified;
A = Cohesive failure of substrate g) the date of the test.

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